Ivanović, Darko

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21857412-bbd9-48e2-a499-af8606835ba3
  • Ivanović, Darko (41)
Projects

Author's Bibliography

Investigation of the retention mechanisms of amlodipine besylate, bisoprolol fumarate, and their impurities on three different HILIC columns

Kasagić-Vujanović, Irena; Jančić-Stojanović, Biljana; Ivanović, Darko

(Taylor & Francis Inc, Philadelphia, 2018)

TY  - JOUR
AU  - Kasagić-Vujanović, Irena
AU  - Jančić-Stojanović, Biljana
AU  - Ivanović, Darko
PY  - 2018
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/3041
AB  - Using theoretical models, retention mechanisms of amlodipine besilate and its impurities D, E, and F were tested, as well as bisoprolol fumarate and its impurities A, C, K, and L. Appropriate theoretical retention models for tested compounds were used, which enabled the determination of retention mechanisms responsible for the separation of tested compounds on three different HILIC column: silica, amino, and diol. In order to describe the effect of ratio of aqueous and organic portion of the mobile phase on the retention behavior of tested compounds, as well as the consideration of shares of partition and adsorption processes in HILIC retention mechanism in all three columns, partitioning and adsorption retention theoretical models were calculated. For this purpose, the water content was varied in the range from 4% to 29%, corresponding to the HILIC region of mobile phase composition. During the experiment, values of other factors of mobile phase were maintained at a constant level. Regression coefficients of partition and adsorption retention models and the corresponding determination coefficients were determined (R-2). Partitioning models for all tested compounds on amino column had higher R-2 values, while adsorption models for all compounds tested on silica and diol column had higher R-2 value. [GRAPHICS] .
PB  - Taylor & Francis Inc, Philadelphia
T2  - Journal of Liquid Chromatography & Related Technologies
T1  - Investigation of the retention mechanisms of amlodipine besylate, bisoprolol fumarate, and their impurities on three different HILIC columns
VL  - 41
IS  - 9
SP  - 523
EP  - 531
DO  - 10.1080/10826076.2018.1476380
ER  - 
@article{
author = "Kasagić-Vujanović, Irena and Jančić-Stojanović, Biljana and Ivanović, Darko",
year = "2018",
abstract = "Using theoretical models, retention mechanisms of amlodipine besilate and its impurities D, E, and F were tested, as well as bisoprolol fumarate and its impurities A, C, K, and L. Appropriate theoretical retention models for tested compounds were used, which enabled the determination of retention mechanisms responsible for the separation of tested compounds on three different HILIC column: silica, amino, and diol. In order to describe the effect of ratio of aqueous and organic portion of the mobile phase on the retention behavior of tested compounds, as well as the consideration of shares of partition and adsorption processes in HILIC retention mechanism in all three columns, partitioning and adsorption retention theoretical models were calculated. For this purpose, the water content was varied in the range from 4% to 29%, corresponding to the HILIC region of mobile phase composition. During the experiment, values of other factors of mobile phase were maintained at a constant level. Regression coefficients of partition and adsorption retention models and the corresponding determination coefficients were determined (R-2). Partitioning models for all tested compounds on amino column had higher R-2 values, while adsorption models for all compounds tested on silica and diol column had higher R-2 value. [GRAPHICS] .",
publisher = "Taylor & Francis Inc, Philadelphia",
journal = "Journal of Liquid Chromatography & Related Technologies",
title = "Investigation of the retention mechanisms of amlodipine besylate, bisoprolol fumarate, and their impurities on three different HILIC columns",
volume = "41",
number = "9",
pages = "523-531",
doi = "10.1080/10826076.2018.1476380"
}
Kasagić-Vujanović, I., Jančić-Stojanović, B.,& Ivanović, D.. (2018). Investigation of the retention mechanisms of amlodipine besylate, bisoprolol fumarate, and their impurities on three different HILIC columns. in Journal of Liquid Chromatography & Related Technologies
Taylor & Francis Inc, Philadelphia., 41(9), 523-531.
https://doi.org/10.1080/10826076.2018.1476380
Kasagić-Vujanović I, Jančić-Stojanović B, Ivanović D. Investigation of the retention mechanisms of amlodipine besylate, bisoprolol fumarate, and their impurities on three different HILIC columns. in Journal of Liquid Chromatography & Related Technologies. 2018;41(9):523-531.
doi:10.1080/10826076.2018.1476380 .
Kasagić-Vujanović, Irena, Jančić-Stojanović, Biljana, Ivanović, Darko, "Investigation of the retention mechanisms of amlodipine besylate, bisoprolol fumarate, and their impurities on three different HILIC columns" in Journal of Liquid Chromatography & Related Technologies, 41, no. 9 (2018):523-531,
https://doi.org/10.1080/10826076.2018.1476380 . .
9
7
9

Monitoring of bisoprolol fumarate stability under different stress conditions

Kasagić-Vujanović, Irena; Jančić-Stojanović, Biljana; Ivanović, Darko

(Springer-Verlag Singapore Pte Ltd, Singapore, 2017)

TY  - CONF
AU  - Kasagić-Vujanović, Irena
AU  - Jančić-Stojanović, Biljana
AU  - Ivanović, Darko
PY  - 2017
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2962
AB  - Stability studies of drugs by stress study is a very important process which is done by treating the study drug with different stress agents, with the aim to define the critical factors affecting the stability of the drug, to accurately define the storage conditions of the drug, as well as to identify the resulting degradation products. In this paper, stress studies of bisoprolol fumarate were performed, in order to examine what are the stress agents that affect its stability. For the analysis previously optimized and validated HILIC method was used It was demonstrated that oxidative stress agent has the largest effect on the degradation of bisoprolol fumarate, and then the acid and base stress agent successively. Water, as a neutral medium, and light had no significant effect on the stability of bisoprolol fumarate. During degradation under acid conditions impurity A was formed and it was confirmed with UPLC/MS/MS method. In order to more clearly define the processes of degradation, kinetic studies of degradation of bisoprolol fumarate have been carried out, in order to determine the order of the reaction rate of degradation and degradation half-time, which provided clearer definition of the mechanism of degradation.
PB  - Springer-Verlag Singapore Pte Ltd, Singapore
C3  - Proceedings of the International Conference on Medical and Biological Engineering 2017 (Cmbebih 2017
T1  - Monitoring of bisoprolol fumarate stability under different stress conditions
VL  - 62
SP  - 415
EP  - 424
DO  - 10.1007/978-981-10-4166-2_64
ER  - 
@conference{
author = "Kasagić-Vujanović, Irena and Jančić-Stojanović, Biljana and Ivanović, Darko",
year = "2017",
abstract = "Stability studies of drugs by stress study is a very important process which is done by treating the study drug with different stress agents, with the aim to define the critical factors affecting the stability of the drug, to accurately define the storage conditions of the drug, as well as to identify the resulting degradation products. In this paper, stress studies of bisoprolol fumarate were performed, in order to examine what are the stress agents that affect its stability. For the analysis previously optimized and validated HILIC method was used It was demonstrated that oxidative stress agent has the largest effect on the degradation of bisoprolol fumarate, and then the acid and base stress agent successively. Water, as a neutral medium, and light had no significant effect on the stability of bisoprolol fumarate. During degradation under acid conditions impurity A was formed and it was confirmed with UPLC/MS/MS method. In order to more clearly define the processes of degradation, kinetic studies of degradation of bisoprolol fumarate have been carried out, in order to determine the order of the reaction rate of degradation and degradation half-time, which provided clearer definition of the mechanism of degradation.",
publisher = "Springer-Verlag Singapore Pte Ltd, Singapore",
journal = "Proceedings of the International Conference on Medical and Biological Engineering 2017 (Cmbebih 2017",
title = "Monitoring of bisoprolol fumarate stability under different stress conditions",
volume = "62",
pages = "415-424",
doi = "10.1007/978-981-10-4166-2_64"
}
Kasagić-Vujanović, I., Jančić-Stojanović, B.,& Ivanović, D.. (2017). Monitoring of bisoprolol fumarate stability under different stress conditions. in Proceedings of the International Conference on Medical and Biological Engineering 2017 (Cmbebih 2017
Springer-Verlag Singapore Pte Ltd, Singapore., 62, 415-424.
https://doi.org/10.1007/978-981-10-4166-2_64
Kasagić-Vujanović I, Jančić-Stojanović B, Ivanović D. Monitoring of bisoprolol fumarate stability under different stress conditions. in Proceedings of the International Conference on Medical and Biological Engineering 2017 (Cmbebih 2017. 2017;62:415-424.
doi:10.1007/978-981-10-4166-2_64 .
Kasagić-Vujanović, Irena, Jančić-Stojanović, Biljana, Ivanović, Darko, "Monitoring of bisoprolol fumarate stability under different stress conditions" in Proceedings of the International Conference on Medical and Biological Engineering 2017 (Cmbebih 2017, 62 (2017):415-424,
https://doi.org/10.1007/978-981-10-4166-2_64 . .
9
2
8

Development of New Liquid Chromatographic Method for Mitotane and Its Metabolites Determination in Human Plasma Employing Design of Experiments Methodology

Jančić-Stojanović, Biljana; Vemić, Sava; Elezović, Valentina; Petrović, Ana; Sinadinović, Zoran; Ivanović, Darko; Damjanović, Svetozar S.; Miljković, Branislava

(Taylor & Francis Inc, Philadelphia, 2015)

TY  - JOUR
AU  - Jančić-Stojanović, Biljana
AU  - Vemić, Sava
AU  - Elezović, Valentina
AU  - Petrović, Ana
AU  - Sinadinović, Zoran
AU  - Ivanović, Darko
AU  - Damjanović, Svetozar S.
AU  - Miljković, Branislava
PY  - 2015
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2438
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/3432
AB  - A simple and reliable new HPLC method with UV detection has been developed and validated for simultaneous determination of mitotane and its two metabolites DDA and DDE. Method development was carried out utilizing systematical approach of the design of experiments (DoE) methodology. For estimation of factors influence on selected chromatographic responses and definition of the optimal chromatographic conditions, Box-Behnken experimental design was applied. The defined optimal separation conditions were: column Restek Ultra Aqua C-18 with pre-column Restek Ultra Aqua C-18 operating at temperature 35 degrees C; mixture of acetonitrile and 0.5% formic acid as mobile phase with 1.2mL min(-1) flow rate and detection at 230nm. As sample preparation method, liquid-liquid extraction was chosen. Method was fully validated and LOQ and LOD were experimentally determined. Finally, method was successfully applied for determination of mitotane and its metabolites in plasma samples of patients with adrenocortical carcinoma.
PB  - Taylor & Francis Inc, Philadelphia
T2  - Journal of Liquid Chromatography & Related Technologies
T1  - Development of New Liquid Chromatographic Method for Mitotane and Its Metabolites Determination in Human Plasma Employing Design of Experiments Methodology
VL  - 38
IS  - 14
SP  - 1371
EP  - 1378
DO  - 10.1080/10826076.2015.1057645
ER  - 
@article{
author = "Jančić-Stojanović, Biljana and Vemić, Sava and Elezović, Valentina and Petrović, Ana and Sinadinović, Zoran and Ivanović, Darko and Damjanović, Svetozar S. and Miljković, Branislava",
year = "2015",
abstract = "A simple and reliable new HPLC method with UV detection has been developed and validated for simultaneous determination of mitotane and its two metabolites DDA and DDE. Method development was carried out utilizing systematical approach of the design of experiments (DoE) methodology. For estimation of factors influence on selected chromatographic responses and definition of the optimal chromatographic conditions, Box-Behnken experimental design was applied. The defined optimal separation conditions were: column Restek Ultra Aqua C-18 with pre-column Restek Ultra Aqua C-18 operating at temperature 35 degrees C; mixture of acetonitrile and 0.5% formic acid as mobile phase with 1.2mL min(-1) flow rate and detection at 230nm. As sample preparation method, liquid-liquid extraction was chosen. Method was fully validated and LOQ and LOD were experimentally determined. Finally, method was successfully applied for determination of mitotane and its metabolites in plasma samples of patients with adrenocortical carcinoma.",
publisher = "Taylor & Francis Inc, Philadelphia",
journal = "Journal of Liquid Chromatography & Related Technologies",
title = "Development of New Liquid Chromatographic Method for Mitotane and Its Metabolites Determination in Human Plasma Employing Design of Experiments Methodology",
volume = "38",
number = "14",
pages = "1371-1378",
doi = "10.1080/10826076.2015.1057645"
}
Jančić-Stojanović, B., Vemić, S., Elezović, V., Petrović, A., Sinadinović, Z., Ivanović, D., Damjanović, S. S.,& Miljković, B.. (2015). Development of New Liquid Chromatographic Method for Mitotane and Its Metabolites Determination in Human Plasma Employing Design of Experiments Methodology. in Journal of Liquid Chromatography & Related Technologies
Taylor & Francis Inc, Philadelphia., 38(14), 1371-1378.
https://doi.org/10.1080/10826076.2015.1057645
Jančić-Stojanović B, Vemić S, Elezović V, Petrović A, Sinadinović Z, Ivanović D, Damjanović SS, Miljković B. Development of New Liquid Chromatographic Method for Mitotane and Its Metabolites Determination in Human Plasma Employing Design of Experiments Methodology. in Journal of Liquid Chromatography & Related Technologies. 2015;38(14):1371-1378.
doi:10.1080/10826076.2015.1057645 .
Jančić-Stojanović, Biljana, Vemić, Sava, Elezović, Valentina, Petrović, Ana, Sinadinović, Zoran, Ivanović, Darko, Damjanović, Svetozar S., Miljković, Branislava, "Development of New Liquid Chromatographic Method for Mitotane and Its Metabolites Determination in Human Plasma Employing Design of Experiments Methodology" in Journal of Liquid Chromatography & Related Technologies, 38, no. 14 (2015):1371-1378,
https://doi.org/10.1080/10826076.2015.1057645 . .
3
2
3

Development of New Liquid Chromatographic Method for Mitotane and Its Metabolites Determination in Human Plasma Employing Design of Experiments Methodology

Jančić-Stojanović, Biljana; Vemić, Sava; Elezović, Valentina; Petrović, Ana; Sinadinović, Zoran; Ivanović, Darko; Damjanović, Svetozar S.; Miljković, Branislava

(Taylor & Francis Inc, Philadelphia, 2015)

TY  - JOUR
AU  - Jančić-Stojanović, Biljana
AU  - Vemić, Sava
AU  - Elezović, Valentina
AU  - Petrović, Ana
AU  - Sinadinović, Zoran
AU  - Ivanović, Darko
AU  - Damjanović, Svetozar S.
AU  - Miljković, Branislava
PY  - 2015
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2438
AB  - A simple and reliable new HPLC method with UV detection has been developed and validated for simultaneous determination of mitotane and its two metabolites DDA and DDE. Method development was carried out utilizing systematical approach of the design of experiments (DoE) methodology. For estimation of factors influence on selected chromatographic responses and definition of the optimal chromatographic conditions, Box-Behnken experimental design was applied. The defined optimal separation conditions were: column Restek Ultra Aqua C-18 with pre-column Restek Ultra Aqua C-18 operating at temperature 35 degrees C; mixture of acetonitrile and 0.5% formic acid as mobile phase with 1.2mL min(-1) flow rate and detection at 230nm. As sample preparation method, liquid-liquid extraction was chosen. Method was fully validated and LOQ and LOD were experimentally determined. Finally, method was successfully applied for determination of mitotane and its metabolites in plasma samples of patients with adrenocortical carcinoma.
PB  - Taylor & Francis Inc, Philadelphia
T2  - Journal of Liquid Chromatography & Related Technologies
T1  - Development of New Liquid Chromatographic Method for Mitotane and Its Metabolites Determination in Human Plasma Employing Design of Experiments Methodology
VL  - 38
IS  - 14
SP  - 1371
EP  - 1378
DO  - 10.1080/10826076.2015.1057645
ER  - 
@article{
author = "Jančić-Stojanović, Biljana and Vemić, Sava and Elezović, Valentina and Petrović, Ana and Sinadinović, Zoran and Ivanović, Darko and Damjanović, Svetozar S. and Miljković, Branislava",
year = "2015",
abstract = "A simple and reliable new HPLC method with UV detection has been developed and validated for simultaneous determination of mitotane and its two metabolites DDA and DDE. Method development was carried out utilizing systematical approach of the design of experiments (DoE) methodology. For estimation of factors influence on selected chromatographic responses and definition of the optimal chromatographic conditions, Box-Behnken experimental design was applied. The defined optimal separation conditions were: column Restek Ultra Aqua C-18 with pre-column Restek Ultra Aqua C-18 operating at temperature 35 degrees C; mixture of acetonitrile and 0.5% formic acid as mobile phase with 1.2mL min(-1) flow rate and detection at 230nm. As sample preparation method, liquid-liquid extraction was chosen. Method was fully validated and LOQ and LOD were experimentally determined. Finally, method was successfully applied for determination of mitotane and its metabolites in plasma samples of patients with adrenocortical carcinoma.",
publisher = "Taylor & Francis Inc, Philadelphia",
journal = "Journal of Liquid Chromatography & Related Technologies",
title = "Development of New Liquid Chromatographic Method for Mitotane and Its Metabolites Determination in Human Plasma Employing Design of Experiments Methodology",
volume = "38",
number = "14",
pages = "1371-1378",
doi = "10.1080/10826076.2015.1057645"
}
Jančić-Stojanović, B., Vemić, S., Elezović, V., Petrović, A., Sinadinović, Z., Ivanović, D., Damjanović, S. S.,& Miljković, B.. (2015). Development of New Liquid Chromatographic Method for Mitotane and Its Metabolites Determination in Human Plasma Employing Design of Experiments Methodology. in Journal of Liquid Chromatography & Related Technologies
Taylor & Francis Inc, Philadelphia., 38(14), 1371-1378.
https://doi.org/10.1080/10826076.2015.1057645
Jančić-Stojanović B, Vemić S, Elezović V, Petrović A, Sinadinović Z, Ivanović D, Damjanović SS, Miljković B. Development of New Liquid Chromatographic Method for Mitotane and Its Metabolites Determination in Human Plasma Employing Design of Experiments Methodology. in Journal of Liquid Chromatography & Related Technologies. 2015;38(14):1371-1378.
doi:10.1080/10826076.2015.1057645 .
Jančić-Stojanović, Biljana, Vemić, Sava, Elezović, Valentina, Petrović, Ana, Sinadinović, Zoran, Ivanović, Darko, Damjanović, Svetozar S., Miljković, Branislava, "Development of New Liquid Chromatographic Method for Mitotane and Its Metabolites Determination in Human Plasma Employing Design of Experiments Methodology" in Journal of Liquid Chromatography & Related Technologies, 38, no. 14 (2015):1371-1378,
https://doi.org/10.1080/10826076.2015.1057645 . .
3
2
3

Optimization of the Separation of Ephedrine, Pseudoephedrine, Phenylephrine, and Synephrine by Hydrophilic Interaction Liquid Chromatography Employing Experimental Design Methodology

Jovanović, Marko; Rakić, Tijana; Ivanović, Darko; Jančić-Stojanović, Biljana

(Taylor & Francis Inc, Philadelphia, 2015)

TY  - JOUR
AU  - Jovanović, Marko
AU  - Rakić, Tijana
AU  - Ivanović, Darko
AU  - Jančić-Stojanović, Biljana
PY  - 2015
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2400
AB  - Hydrophilic interaction liquid chromatography (HILIC) has emerged as an alternative separation technique for small polar compounds. Design of Experiments (DoE) methodology in the analysis of the retention behavior and method development have been shown to be successful. This article addresses the retention behavior and optimization of chromatographic separation of a model mixture consisting of four sympathomimetic drugs (ephedrine, pseudoephedrine, phenylephrine, synephrine), on a bare silica column by HILIC. The acetonitrile content, pH of the aqueous phase, and concentration of ammonium acetate in aqueous phase were optimized according to the matrix of Box-Behnken design, and retention data were fitted to second-order polynomial models. The obtained coefficients of determination R-2 were higher than 0.990 and adjusted R-2 exceeded 0.972, while the lowest value for Predicted R-2 was 0.845. Beside of statistical analysis, graphical estimation of retention behavior was performed. In order to optimize the separation, indirect modeling of selectivity factors of critical peak pairs (the diastereoisomers ephedrine/pseudoephedrine and the positional isomers phenylephrine/synephrine) and grid point search approach were employed. After the development of the grids, optimal chromatographic conditions were selected (acetonitrile content 91%, pH of the aqueous phase 4.5 and ammonium acetate concetration 35mmolL(-1)), providing a total analysis time of 14min.
PB  - Taylor & Francis Inc, Philadelphia
T2  - Instrumentation Science & Technology
T1  - Optimization of the Separation of Ephedrine, Pseudoephedrine, Phenylephrine, and Synephrine by Hydrophilic Interaction Liquid Chromatography Employing Experimental Design Methodology
VL  - 43
IS  - 2
SP  - 156
EP  - 169
DO  - 10.1080/10739149.2014.910670
ER  - 
@article{
author = "Jovanović, Marko and Rakić, Tijana and Ivanović, Darko and Jančić-Stojanović, Biljana",
year = "2015",
abstract = "Hydrophilic interaction liquid chromatography (HILIC) has emerged as an alternative separation technique for small polar compounds. Design of Experiments (DoE) methodology in the analysis of the retention behavior and method development have been shown to be successful. This article addresses the retention behavior and optimization of chromatographic separation of a model mixture consisting of four sympathomimetic drugs (ephedrine, pseudoephedrine, phenylephrine, synephrine), on a bare silica column by HILIC. The acetonitrile content, pH of the aqueous phase, and concentration of ammonium acetate in aqueous phase were optimized according to the matrix of Box-Behnken design, and retention data were fitted to second-order polynomial models. The obtained coefficients of determination R-2 were higher than 0.990 and adjusted R-2 exceeded 0.972, while the lowest value for Predicted R-2 was 0.845. Beside of statistical analysis, graphical estimation of retention behavior was performed. In order to optimize the separation, indirect modeling of selectivity factors of critical peak pairs (the diastereoisomers ephedrine/pseudoephedrine and the positional isomers phenylephrine/synephrine) and grid point search approach were employed. After the development of the grids, optimal chromatographic conditions were selected (acetonitrile content 91%, pH of the aqueous phase 4.5 and ammonium acetate concetration 35mmolL(-1)), providing a total analysis time of 14min.",
publisher = "Taylor & Francis Inc, Philadelphia",
journal = "Instrumentation Science & Technology",
title = "Optimization of the Separation of Ephedrine, Pseudoephedrine, Phenylephrine, and Synephrine by Hydrophilic Interaction Liquid Chromatography Employing Experimental Design Methodology",
volume = "43",
number = "2",
pages = "156-169",
doi = "10.1080/10739149.2014.910670"
}
Jovanović, M., Rakić, T., Ivanović, D.,& Jančić-Stojanović, B.. (2015). Optimization of the Separation of Ephedrine, Pseudoephedrine, Phenylephrine, and Synephrine by Hydrophilic Interaction Liquid Chromatography Employing Experimental Design Methodology. in Instrumentation Science & Technology
Taylor & Francis Inc, Philadelphia., 43(2), 156-169.
https://doi.org/10.1080/10739149.2014.910670
Jovanović M, Rakić T, Ivanović D, Jančić-Stojanović B. Optimization of the Separation of Ephedrine, Pseudoephedrine, Phenylephrine, and Synephrine by Hydrophilic Interaction Liquid Chromatography Employing Experimental Design Methodology. in Instrumentation Science & Technology. 2015;43(2):156-169.
doi:10.1080/10739149.2014.910670 .
Jovanović, Marko, Rakić, Tijana, Ivanović, Darko, Jančić-Stojanović, Biljana, "Optimization of the Separation of Ephedrine, Pseudoephedrine, Phenylephrine, and Synephrine by Hydrophilic Interaction Liquid Chromatography Employing Experimental Design Methodology" in Instrumentation Science & Technology, 43, no. 2 (2015):156-169,
https://doi.org/10.1080/10739149.2014.910670 . .
6
3
7

Design of Experiments in Optimization and Validation of a Hydrophilic Interaction Liquid Chromatography Method for Determination of Amlodipine Besylate and Bisoprolol Fumarate

Kasagić-Vujanović, Irena; Jančić-Stojanović, Biljana; Rakić, Tijana; Ivanović, Darko

(Taylor & Francis Inc, Philadelphia, 2015)

TY  - JOUR
AU  - Kasagić-Vujanović, Irena
AU  - Jančić-Stojanović, Biljana
AU  - Rakić, Tijana
AU  - Ivanović, Darko
PY  - 2015
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2392
AB  - In this paper chemometrically-assisted optimization and validation of hydrophilic interaction liquid chromatographic (HILIC) method for the quantitative analysis of amlodipine besylate (AB) and bisoprolol fumarate (BF) in pharmaceuticals are presented. In this study, the development of HILIC method for AB and BF separation was performed by a systematic approach which included Design of Experiments (DoE) methodology. First, in method optimization, a central composite design was applied. Influence of the acetonitrile content in the mobile phase, pH of the aqueous phase, and concentration of ammonium acetate on selected chromatographic responses was investigated. Optimal chromatographic conditions in terms of adequate separation and minimal analysis duration were set by graphical optimization overlapping the contour plots as: acetonitrile-water phase (10mM ammonium acetate, pH 4.0 adjusted with glacial acetic acid) (92:8, v/v), column Luna HILIC 200 A, 150mmx4.6mm, 5 mu m particle size, column temperature 30 degrees C, flow rate 1mL min(-1), and UV detection at 230nm. After this step, method robustness was tested using a 2(5-1) fractional factorial design. Statistical and graphical evaluation of results confirmed robustness of the method and then the method was fully validated. Finally, the proposed method was successfully applied for AB and BF determination in pharmaceuticals.
PB  - Taylor & Francis Inc, Philadelphia
T2  - Journal of Liquid Chromatography & Related Technologies
T1  - Design of Experiments in Optimization and Validation of a Hydrophilic Interaction Liquid Chromatography Method for Determination of Amlodipine Besylate and Bisoprolol Fumarate
VL  - 38
IS  - 8
SP  - 919
EP  - 928
DO  - 10.1080/10826076.2014.991872
ER  - 
@article{
author = "Kasagić-Vujanović, Irena and Jančić-Stojanović, Biljana and Rakić, Tijana and Ivanović, Darko",
year = "2015",
abstract = "In this paper chemometrically-assisted optimization and validation of hydrophilic interaction liquid chromatographic (HILIC) method for the quantitative analysis of amlodipine besylate (AB) and bisoprolol fumarate (BF) in pharmaceuticals are presented. In this study, the development of HILIC method for AB and BF separation was performed by a systematic approach which included Design of Experiments (DoE) methodology. First, in method optimization, a central composite design was applied. Influence of the acetonitrile content in the mobile phase, pH of the aqueous phase, and concentration of ammonium acetate on selected chromatographic responses was investigated. Optimal chromatographic conditions in terms of adequate separation and minimal analysis duration were set by graphical optimization overlapping the contour plots as: acetonitrile-water phase (10mM ammonium acetate, pH 4.0 adjusted with glacial acetic acid) (92:8, v/v), column Luna HILIC 200 A, 150mmx4.6mm, 5 mu m particle size, column temperature 30 degrees C, flow rate 1mL min(-1), and UV detection at 230nm. After this step, method robustness was tested using a 2(5-1) fractional factorial design. Statistical and graphical evaluation of results confirmed robustness of the method and then the method was fully validated. Finally, the proposed method was successfully applied for AB and BF determination in pharmaceuticals.",
publisher = "Taylor & Francis Inc, Philadelphia",
journal = "Journal of Liquid Chromatography & Related Technologies",
title = "Design of Experiments in Optimization and Validation of a Hydrophilic Interaction Liquid Chromatography Method for Determination of Amlodipine Besylate and Bisoprolol Fumarate",
volume = "38",
number = "8",
pages = "919-928",
doi = "10.1080/10826076.2014.991872"
}
Kasagić-Vujanović, I., Jančić-Stojanović, B., Rakić, T.,& Ivanović, D.. (2015). Design of Experiments in Optimization and Validation of a Hydrophilic Interaction Liquid Chromatography Method for Determination of Amlodipine Besylate and Bisoprolol Fumarate. in Journal of Liquid Chromatography & Related Technologies
Taylor & Francis Inc, Philadelphia., 38(8), 919-928.
https://doi.org/10.1080/10826076.2014.991872
Kasagić-Vujanović I, Jančić-Stojanović B, Rakić T, Ivanović D. Design of Experiments in Optimization and Validation of a Hydrophilic Interaction Liquid Chromatography Method for Determination of Amlodipine Besylate and Bisoprolol Fumarate. in Journal of Liquid Chromatography & Related Technologies. 2015;38(8):919-928.
doi:10.1080/10826076.2014.991872 .
Kasagić-Vujanović, Irena, Jančić-Stojanović, Biljana, Rakić, Tijana, Ivanović, Darko, "Design of Experiments in Optimization and Validation of a Hydrophilic Interaction Liquid Chromatography Method for Determination of Amlodipine Besylate and Bisoprolol Fumarate" in Journal of Liquid Chromatography & Related Technologies, 38, no. 8 (2015):919-928,
https://doi.org/10.1080/10826076.2014.991872 . .
14
12
15

Chromatographic Analysis of Olopatadine in Hydrophilic Interaction Liquid Chromatography

Maksić, Jelena; Jovanović, Marko; Rakić, Tijana; Popović, Igor; Ivanović, Darko; Jančić-Stojanović, Biljana

(Oxford Univ Press Inc, Cary, 2015)

TY  - JOUR
AU  - Maksić, Jelena
AU  - Jovanović, Marko
AU  - Rakić, Tijana
AU  - Popović, Igor
AU  - Ivanović, Darko
AU  - Jančić-Stojanović, Biljana
PY  - 2015
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2318
AB  - In this paper, chromatographic analysis of active substance olopatadine hydrochloride, which is used in eye drops as antihistaminic agent, and its impurity E isomer by hydrophilic interaction liquid chromatography (HILIC) and application of design of experiments (DoE) methodology are presented. In addition, benzalkonium chloride is very often used as a preservative in eye drops. Therefore, the evaluation of its chromatographic behavior in HILIC was carried out as well. In order to estimate chromatographic behavior and set optimal chromatographic conditions, DoE methodology was applied. After the selection of important chromatographic factors, Box-Behnken design was utilized, and on the basis of the obtained models factor effects were examined. Then, multi-objective robust optimization is performed aiming to obtain chromatographic conditions that comply with several quality criteria simultaneously: adequate and robust separation of critical peak pair and maximum retention of the first eluting peak. The optimal conditions are identified by using grid point search methodology. The experimental verification confirmed the adequacy of the defined optimal conditions. Finally, under optimal chromatographic conditions, the method was validated and applicability of the proposed method was confirmed.
PB  - Oxford Univ Press Inc, Cary
T2  - Journal of Chromatographic Science
T1  - Chromatographic Analysis of Olopatadine in Hydrophilic Interaction Liquid Chromatography
VL  - 53
IS  - 5
SP  - 680
EP  - 686
DO  - 10.1093/chromsci/bmu102
ER  - 
@article{
author = "Maksić, Jelena and Jovanović, Marko and Rakić, Tijana and Popović, Igor and Ivanović, Darko and Jančić-Stojanović, Biljana",
year = "2015",
abstract = "In this paper, chromatographic analysis of active substance olopatadine hydrochloride, which is used in eye drops as antihistaminic agent, and its impurity E isomer by hydrophilic interaction liquid chromatography (HILIC) and application of design of experiments (DoE) methodology are presented. In addition, benzalkonium chloride is very often used as a preservative in eye drops. Therefore, the evaluation of its chromatographic behavior in HILIC was carried out as well. In order to estimate chromatographic behavior and set optimal chromatographic conditions, DoE methodology was applied. After the selection of important chromatographic factors, Box-Behnken design was utilized, and on the basis of the obtained models factor effects were examined. Then, multi-objective robust optimization is performed aiming to obtain chromatographic conditions that comply with several quality criteria simultaneously: adequate and robust separation of critical peak pair and maximum retention of the first eluting peak. The optimal conditions are identified by using grid point search methodology. The experimental verification confirmed the adequacy of the defined optimal conditions. Finally, under optimal chromatographic conditions, the method was validated and applicability of the proposed method was confirmed.",
publisher = "Oxford Univ Press Inc, Cary",
journal = "Journal of Chromatographic Science",
title = "Chromatographic Analysis of Olopatadine in Hydrophilic Interaction Liquid Chromatography",
volume = "53",
number = "5",
pages = "680-686",
doi = "10.1093/chromsci/bmu102"
}
Maksić, J., Jovanović, M., Rakić, T., Popović, I., Ivanović, D.,& Jančić-Stojanović, B.. (2015). Chromatographic Analysis of Olopatadine in Hydrophilic Interaction Liquid Chromatography. in Journal of Chromatographic Science
Oxford Univ Press Inc, Cary., 53(5), 680-686.
https://doi.org/10.1093/chromsci/bmu102
Maksić J, Jovanović M, Rakić T, Popović I, Ivanović D, Jančić-Stojanović B. Chromatographic Analysis of Olopatadine in Hydrophilic Interaction Liquid Chromatography. in Journal of Chromatographic Science. 2015;53(5):680-686.
doi:10.1093/chromsci/bmu102 .
Maksić, Jelena, Jovanović, Marko, Rakić, Tijana, Popović, Igor, Ivanović, Darko, Jančić-Stojanović, Biljana, "Chromatographic Analysis of Olopatadine in Hydrophilic Interaction Liquid Chromatography" in Journal of Chromatographic Science, 53, no. 5 (2015):680-686,
https://doi.org/10.1093/chromsci/bmu102 . .
8
4
9

Determination of pseudoephedrine, paracetamole and ascorbic acid in multicomponent powder using reversed-phase chromatographic method

Malenović, Anđelija; Jančić-Stojanović, Biljana; Ivanović, Darko

(Savez farmaceutskih udruženja Srbije, Beograd, 2014)

TY  - JOUR
AU  - Malenović, Anđelija
AU  - Jančić-Stojanović, Biljana
AU  - Ivanović, Darko
PY  - 2014
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2293
AB  - For the simultaneous analysis of multicomponent mixture containing pseudoephedrine, paracetamole and ascorbic acid two RP-HPLC methods were developed. Separation were performed on Hewlett Packard 1100 system which consisted of HP 1100 binary pump, HP 1100 UV/VIS detector and HP ChemStation for the automatic data evaluation. Methods were developed, e. g. chromatographic conditiond settled, methods submited to method validation and then applied for the determination of content of multicomponent powder.The best separation was achived on Platinium Alltech Amino 150 x 4.6 mm, 5 mm particle size column, at 30°C. Injection volume was 20mL. Mobile phase in mehtod I was a mixture of methanol-water (30:70 V/V), pH 2.5, and in mehtod II was a mixture methanol-water (60:40 V/V), pH 2.9. pH of the mobile phases were adjusted with 85% ortophosphoric acid. Detection was performed at 214 nm in mehtod I and at 257 nm in method II. Flow rate was 1 mLmin-1. Developed methods were validated. Obtained results showed that both methods are suitable for routine analysis of pharmaceutical dosage forms which contain pseudoephedrine, paracetamole and ascorbic acid.
AB  - Za istovremenu analizu trokomponentne smeše koja sadrži pseudoefedrin, paracetamol i askorbinsku kiselinu postavljene su dve metode reverzno-fazne tečne hromatografije pod visokim pritiskom (RP-HPLC). Hromatografski sistem Hewlett Packard 1100 koji čini HP 1100 binarna pumpa, HP 1100 UV-VIS detektor i HP ChemStation za automatsku obradu podataka korišćen je za hromatografsko razdvajanje. Postupak je obuhvatio definisanje hromatografskih uslova, validaciju postavljenih metoda, kao i njihovu primenu za ispitivanje sadržaja pseudoefedrina, paracetamola i askorbinske kiseline u peroralnom prašku. Optimalna separacija postignuta je u koloni Platinium Alltech Amino 150 mm x 4,6 mm, 5 mm veličine čestica, na temperaturi kolone od 30°C. Volumen injektovanja bio je 20 mL. Mobilna faza u metodi I bila je smeša metanol-voda (30:70 V/V), pH vrednost podešena na 2,5, a u metodi II smeša metanol-voda (60:40 V/V), pH vrednost podešena na 2,9. pH mobilne faze je podešavan sa 85%-tnom orto-fosfornom kiselinom. Talasna dužina detekcije bila je 214 nm u metodi I i 257 nm u metodi II. Protok mobilne faze za obe metode bio je 1 mL min-1. Postavljene metode su validirane i na osnovu dobijenih parametara procenjeno je da obe predložene metode mogu da se primene za analizu peroralnog praška koji sadrži paracetamol, pseudoefedrin i askorbinsku kiselinu.
PB  - Savez farmaceutskih udruženja Srbije, Beograd
T2  - Arhiv za farmaciju
T1  - Determination of pseudoephedrine, paracetamole and ascorbic acid in multicomponent powder using reversed-phase chromatographic method
T1  - Određivanje sadržaja pseudoefedrina, paracetamola i askorbinske kiseline u peroralnom prašku primenom reverzno-fazne tečne hromatografije
VL  - 64
IS  - 6
SP  - 473
EP  - 486
DO  - 10.5937/arhfarm1406473M
ER  - 
@article{
author = "Malenović, Anđelija and Jančić-Stojanović, Biljana and Ivanović, Darko",
year = "2014",
abstract = "For the simultaneous analysis of multicomponent mixture containing pseudoephedrine, paracetamole and ascorbic acid two RP-HPLC methods were developed. Separation were performed on Hewlett Packard 1100 system which consisted of HP 1100 binary pump, HP 1100 UV/VIS detector and HP ChemStation for the automatic data evaluation. Methods were developed, e. g. chromatographic conditiond settled, methods submited to method validation and then applied for the determination of content of multicomponent powder.The best separation was achived on Platinium Alltech Amino 150 x 4.6 mm, 5 mm particle size column, at 30°C. Injection volume was 20mL. Mobile phase in mehtod I was a mixture of methanol-water (30:70 V/V), pH 2.5, and in mehtod II was a mixture methanol-water (60:40 V/V), pH 2.9. pH of the mobile phases were adjusted with 85% ortophosphoric acid. Detection was performed at 214 nm in mehtod I and at 257 nm in method II. Flow rate was 1 mLmin-1. Developed methods were validated. Obtained results showed that both methods are suitable for routine analysis of pharmaceutical dosage forms which contain pseudoephedrine, paracetamole and ascorbic acid., Za istovremenu analizu trokomponentne smeše koja sadrži pseudoefedrin, paracetamol i askorbinsku kiselinu postavljene su dve metode reverzno-fazne tečne hromatografije pod visokim pritiskom (RP-HPLC). Hromatografski sistem Hewlett Packard 1100 koji čini HP 1100 binarna pumpa, HP 1100 UV-VIS detektor i HP ChemStation za automatsku obradu podataka korišćen je za hromatografsko razdvajanje. Postupak je obuhvatio definisanje hromatografskih uslova, validaciju postavljenih metoda, kao i njihovu primenu za ispitivanje sadržaja pseudoefedrina, paracetamola i askorbinske kiseline u peroralnom prašku. Optimalna separacija postignuta je u koloni Platinium Alltech Amino 150 mm x 4,6 mm, 5 mm veličine čestica, na temperaturi kolone od 30°C. Volumen injektovanja bio je 20 mL. Mobilna faza u metodi I bila je smeša metanol-voda (30:70 V/V), pH vrednost podešena na 2,5, a u metodi II smeša metanol-voda (60:40 V/V), pH vrednost podešena na 2,9. pH mobilne faze je podešavan sa 85%-tnom orto-fosfornom kiselinom. Talasna dužina detekcije bila je 214 nm u metodi I i 257 nm u metodi II. Protok mobilne faze za obe metode bio je 1 mL min-1. Postavljene metode su validirane i na osnovu dobijenih parametara procenjeno je da obe predložene metode mogu da se primene za analizu peroralnog praška koji sadrži paracetamol, pseudoefedrin i askorbinsku kiselinu.",
publisher = "Savez farmaceutskih udruženja Srbije, Beograd",
journal = "Arhiv za farmaciju",
title = "Determination of pseudoephedrine, paracetamole and ascorbic acid in multicomponent powder using reversed-phase chromatographic method, Određivanje sadržaja pseudoefedrina, paracetamola i askorbinske kiseline u peroralnom prašku primenom reverzno-fazne tečne hromatografije",
volume = "64",
number = "6",
pages = "473-486",
doi = "10.5937/arhfarm1406473M"
}
Malenović, A., Jančić-Stojanović, B.,& Ivanović, D.. (2014). Determination of pseudoephedrine, paracetamole and ascorbic acid in multicomponent powder using reversed-phase chromatographic method. in Arhiv za farmaciju
Savez farmaceutskih udruženja Srbije, Beograd., 64(6), 473-486.
https://doi.org/10.5937/arhfarm1406473M
Malenović A, Jančić-Stojanović B, Ivanović D. Determination of pseudoephedrine, paracetamole and ascorbic acid in multicomponent powder using reversed-phase chromatographic method. in Arhiv za farmaciju. 2014;64(6):473-486.
doi:10.5937/arhfarm1406473M .
Malenović, Anđelija, Jančić-Stojanović, Biljana, Ivanović, Darko, "Determination of pseudoephedrine, paracetamole and ascorbic acid in multicomponent powder using reversed-phase chromatographic method" in Arhiv za farmaciju, 64, no. 6 (2014):473-486,
https://doi.org/10.5937/arhfarm1406473M . .

Development of chromatographic methods for analysis of sulfamethoxazole, trimethoprim, their degradation products and preservatives in syrup

Perović, Ivana; Malenović, Anđelija; Vemić, Ana; Kostić, Nađa; Ivanović, Darko

(Savez farmaceutskih udruženja Srbije, Beograd, 2014)

TY  - JOUR
AU  - Perović, Ivana
AU  - Malenović, Anđelija
AU  - Vemić, Ana
AU  - Kostić, Nađa
AU  - Ivanović, Darko
PY  - 2014
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2242
AB  - In this paper the experimental conditions for optimal reversed-phase liquid chromatographic (RP-HPLC) determination of sulfamethoxazole, trimethoprim and preservatives, as well as degradation products of sulfamethoxazole and trimethoprim in syrup were defined. The determination of active compounds and preservatives was carried out on Zorbax Eclipse XDB-C18, 150 mm × 4.6 mm, 5 μm particle size column, mobile phase flow rate was 1.5 mL min-1, and detection at 235 nm for the active compounds and 254 nm for preservatives. Mobile phase A consisted of 150 mL of acetonitrile, 850 mL of water and 1 mL of triethanolamine (pH 5.90 adjusted with diluted acetic acid), while mobile phase B was acetonitrile. The mobile phase ratio was defined by the gradient program. For the determination of degradation products Zorbax Eclipse Plus C18, 100 mm x 4.6 mm, 3.5 μm particle size column was used, the mobile phase flow rate was 0.5 mL min-1 and detection at 210 nm for 3,4,5-trimethoxybenzoic acid and 254 nm for sulfanilic acid and sulfanilamide. Mobile phase A was 50 mM potassium dihydrogenphosphate (pH 5.60 adjusted with a 0.5 mol L-1 potassium hydroxide), while mobile phase B was acetonitrile. The mobile phase ratio was defined by the gradient program. Through the validation of the developed methods their efficiency and reliability is confirmed and consequently the adequacy for the routine control.
AB  - U ovom radu prikazano je definisanje eksperimentalnih uslova i optimizacija metoda reverzno-fazne tečne hromatografije (RP-HPLC) za određivanje sulfametoksazola, trimetoprima i konzervanasa, odnosno degradacionih proizvoda sulfametoksazola i trimetoprima u sirupu. Određivanje sadržaja aktivnih komponenti i konzervanasa vršeno je na koloni Zorbax Eclipse XDB-C18, 150 mm × 4,6 mm, 5 μm veličine čestica, protok mobilne faze bio je 1,5 mL min-1, dok je detekcija vršena na 235 nm za aktivne komponente i 254 nm za konzervanse. Mobilna faza A sastojala se od smeše 150 mL acetonitrila, 850 mL vode i 1 mL trietanolamina (pH 5,9 podešen razblaženom sirćetnom kiselinom), a kao mobilna faza B korišćen je acetonitril. Odnos mobilnih faza tokom analize definisan je programom gradijenta. Određivanje sadržaja degradacionih proizvoda vršeno je na koloni Zorbax Eclipse Plus-C18, 100 mm × 4,6 mm, 3,5 μm veličine čestica, uz protok mobilne faze od 0,5 mL min-1 i detekciju na 210 nm za 3,4,5-trimetoksibenzojevu kiselinu i 254 nm za sulfanilnu kiselinu i sulfanilamid. Mobilna faza A bila je 50 mM kalijum-dihidrogenfosfat (pH 5,60 podešen sa 0,5 mol L-1 kalijum-hidroksidom), a mobilna faza B bio je acetonitril. Odnos mobilnih faza tokom analize definisan je programom gradijenta. Validacijom postavljenih metoda potvrđeno je da su efikasne i pouzdane, i kao takve pogodne za rutinsku kontrolu.
PB  - Savez farmaceutskih udruženja Srbije, Beograd
T2  - Arhiv za farmaciju
T1  - Development of chromatographic methods for analysis of sulfamethoxazole, trimethoprim, their degradation products and preservatives in syrup
T1  - Razvoj hromatografskih metoda za analizu sulfametoksazola, trimetoprima, njihovih degradacionih proizvoda i konzervanasa u sirupu
VL  - 64
IS  - 2
SP  - 112
EP  - 127
DO  - 10.5937/arhfarm1402112P
ER  - 
@article{
author = "Perović, Ivana and Malenović, Anđelija and Vemić, Ana and Kostić, Nađa and Ivanović, Darko",
year = "2014",
abstract = "In this paper the experimental conditions for optimal reversed-phase liquid chromatographic (RP-HPLC) determination of sulfamethoxazole, trimethoprim and preservatives, as well as degradation products of sulfamethoxazole and trimethoprim in syrup were defined. The determination of active compounds and preservatives was carried out on Zorbax Eclipse XDB-C18, 150 mm × 4.6 mm, 5 μm particle size column, mobile phase flow rate was 1.5 mL min-1, and detection at 235 nm for the active compounds and 254 nm for preservatives. Mobile phase A consisted of 150 mL of acetonitrile, 850 mL of water and 1 mL of triethanolamine (pH 5.90 adjusted with diluted acetic acid), while mobile phase B was acetonitrile. The mobile phase ratio was defined by the gradient program. For the determination of degradation products Zorbax Eclipse Plus C18, 100 mm x 4.6 mm, 3.5 μm particle size column was used, the mobile phase flow rate was 0.5 mL min-1 and detection at 210 nm for 3,4,5-trimethoxybenzoic acid and 254 nm for sulfanilic acid and sulfanilamide. Mobile phase A was 50 mM potassium dihydrogenphosphate (pH 5.60 adjusted with a 0.5 mol L-1 potassium hydroxide), while mobile phase B was acetonitrile. The mobile phase ratio was defined by the gradient program. Through the validation of the developed methods their efficiency and reliability is confirmed and consequently the adequacy for the routine control., U ovom radu prikazano je definisanje eksperimentalnih uslova i optimizacija metoda reverzno-fazne tečne hromatografije (RP-HPLC) za određivanje sulfametoksazola, trimetoprima i konzervanasa, odnosno degradacionih proizvoda sulfametoksazola i trimetoprima u sirupu. Određivanje sadržaja aktivnih komponenti i konzervanasa vršeno je na koloni Zorbax Eclipse XDB-C18, 150 mm × 4,6 mm, 5 μm veličine čestica, protok mobilne faze bio je 1,5 mL min-1, dok je detekcija vršena na 235 nm za aktivne komponente i 254 nm za konzervanse. Mobilna faza A sastojala se od smeše 150 mL acetonitrila, 850 mL vode i 1 mL trietanolamina (pH 5,9 podešen razblaženom sirćetnom kiselinom), a kao mobilna faza B korišćen je acetonitril. Odnos mobilnih faza tokom analize definisan je programom gradijenta. Određivanje sadržaja degradacionih proizvoda vršeno je na koloni Zorbax Eclipse Plus-C18, 100 mm × 4,6 mm, 3,5 μm veličine čestica, uz protok mobilne faze od 0,5 mL min-1 i detekciju na 210 nm za 3,4,5-trimetoksibenzojevu kiselinu i 254 nm za sulfanilnu kiselinu i sulfanilamid. Mobilna faza A bila je 50 mM kalijum-dihidrogenfosfat (pH 5,60 podešen sa 0,5 mol L-1 kalijum-hidroksidom), a mobilna faza B bio je acetonitril. Odnos mobilnih faza tokom analize definisan je programom gradijenta. Validacijom postavljenih metoda potvrđeno je da su efikasne i pouzdane, i kao takve pogodne za rutinsku kontrolu.",
publisher = "Savez farmaceutskih udruženja Srbije, Beograd",
journal = "Arhiv za farmaciju",
title = "Development of chromatographic methods for analysis of sulfamethoxazole, trimethoprim, their degradation products and preservatives in syrup, Razvoj hromatografskih metoda za analizu sulfametoksazola, trimetoprima, njihovih degradacionih proizvoda i konzervanasa u sirupu",
volume = "64",
number = "2",
pages = "112-127",
doi = "10.5937/arhfarm1402112P"
}
Perović, I., Malenović, A., Vemić, A., Kostić, N.,& Ivanović, D.. (2014). Development of chromatographic methods for analysis of sulfamethoxazole, trimethoprim, their degradation products and preservatives in syrup. in Arhiv za farmaciju
Savez farmaceutskih udruženja Srbije, Beograd., 64(2), 112-127.
https://doi.org/10.5937/arhfarm1402112P
Perović I, Malenović A, Vemić A, Kostić N, Ivanović D. Development of chromatographic methods for analysis of sulfamethoxazole, trimethoprim, their degradation products and preservatives in syrup. in Arhiv za farmaciju. 2014;64(2):112-127.
doi:10.5937/arhfarm1402112P .
Perović, Ivana, Malenović, Anđelija, Vemić, Ana, Kostić, Nađa, Ivanović, Darko, "Development of chromatographic methods for analysis of sulfamethoxazole, trimethoprim, their degradation products and preservatives in syrup" in Arhiv za farmaciju, 64, no. 2 (2014):112-127,
https://doi.org/10.5937/arhfarm1402112P . .
1

Study of forced degradation of amlodipine besylate and bisoprolol fumarate by application of hydrophilic interaction liquid chromatography

Kasagić-Vujanović, Irena; Jančić-Stojanović, Biljana; Ivanović, Darko

(Savez farmaceutskih udruženja Srbije, Beograd, 2014)

TY  - JOUR
AU  - Kasagić-Vujanović, Irena
AU  - Jančić-Stojanović, Biljana
AU  - Ivanović, Darko
PY  - 2014
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2282
AB  - Currently, in pharmaceutical analysis, great importance is given to forced degradation studies, which can greatly help to predict the shelf life of the drug, but also for identification of possible degradation products. These studies enable investigation of stability indicating method, then it is used to test the active substances intrinsic/inner molecular stability, as well as defining active substances impurity profiles. In this work forced degradation studies of amlodipine besylate and bisoprolol fumarate either individually and in mixtures, was performed, where the method of hydrophilic interaction liquid chromatography was used, and any possible changes in the concentration of samples were followed. The results showed that the test compounds are sensitive to the tested stress agents, especially amlodipine besylate, and that both of these compounds showed increased stability in the mixture in comparison to individual analysis.
AB  - U savremenim farmaceutskim analizama danas se veliki značaj pridaje studijama forsirane degradacije, koje mogu u velikoj mjeri pomoći u predviđanju roka upotrebe lijeka, ali i u identifikaciji mogućih proizvoda degradacije. Ove studije omogućavaju ispitivanje specifičnosti stability indicating metode, zatim koriste se za ispitivanje intrinzičke/unutrašnje stabilnosti molekule aktivnih supstanci, kao i za definisanje profila nečistoća aktivnih supstanci. U ovom radu vršena je studija forsirane degradacije amlodipin-besilata i bisoprolol-fumarata pojedinačno i u smješi, gdje se kao metoda koristila tečna hromatografija hidrofilnih interakcija, kojom su se pratile promjene koncentracije ispitivanih uzoraka. Rezultati ispitivanja pokazali su da su ispitivana jedinjenja osjetljiva na većinu ispitivanih stres agenasa, naročito amlodipinbesilat, kao i da su oba ova jedinjenja pokazala veću stabilnost u smješi, nego kad su pojedinačno analizirana.
PB  - Savez farmaceutskih udruženja Srbije, Beograd
T2  - Arhiv za farmaciju
T1  - Study of forced degradation of amlodipine besylate and bisoprolol fumarate by application of hydrophilic interaction liquid chromatography
T1  - Studije forsirane degradacije amlodipin-besilata i bisoprolol-fumarata primjenom tečne hromatografije hidrofilnih interakcija
VL  - 64
IS  - 3
SP  - 230
EP  - 246
DO  - 10.5937/arhfarm1403230K
ER  - 
@article{
author = "Kasagić-Vujanović, Irena and Jančić-Stojanović, Biljana and Ivanović, Darko",
year = "2014",
abstract = "Currently, in pharmaceutical analysis, great importance is given to forced degradation studies, which can greatly help to predict the shelf life of the drug, but also for identification of possible degradation products. These studies enable investigation of stability indicating method, then it is used to test the active substances intrinsic/inner molecular stability, as well as defining active substances impurity profiles. In this work forced degradation studies of amlodipine besylate and bisoprolol fumarate either individually and in mixtures, was performed, where the method of hydrophilic interaction liquid chromatography was used, and any possible changes in the concentration of samples were followed. The results showed that the test compounds are sensitive to the tested stress agents, especially amlodipine besylate, and that both of these compounds showed increased stability in the mixture in comparison to individual analysis., U savremenim farmaceutskim analizama danas se veliki značaj pridaje studijama forsirane degradacije, koje mogu u velikoj mjeri pomoći u predviđanju roka upotrebe lijeka, ali i u identifikaciji mogućih proizvoda degradacije. Ove studije omogućavaju ispitivanje specifičnosti stability indicating metode, zatim koriste se za ispitivanje intrinzičke/unutrašnje stabilnosti molekule aktivnih supstanci, kao i za definisanje profila nečistoća aktivnih supstanci. U ovom radu vršena je studija forsirane degradacije amlodipin-besilata i bisoprolol-fumarata pojedinačno i u smješi, gdje se kao metoda koristila tečna hromatografija hidrofilnih interakcija, kojom su se pratile promjene koncentracije ispitivanih uzoraka. Rezultati ispitivanja pokazali su da su ispitivana jedinjenja osjetljiva na većinu ispitivanih stres agenasa, naročito amlodipinbesilat, kao i da su oba ova jedinjenja pokazala veću stabilnost u smješi, nego kad su pojedinačno analizirana.",
publisher = "Savez farmaceutskih udruženja Srbije, Beograd",
journal = "Arhiv za farmaciju",
title = "Study of forced degradation of amlodipine besylate and bisoprolol fumarate by application of hydrophilic interaction liquid chromatography, Studije forsirane degradacije amlodipin-besilata i bisoprolol-fumarata primjenom tečne hromatografije hidrofilnih interakcija",
volume = "64",
number = "3",
pages = "230-246",
doi = "10.5937/arhfarm1403230K"
}
Kasagić-Vujanović, I., Jančić-Stojanović, B.,& Ivanović, D.. (2014). Study of forced degradation of amlodipine besylate and bisoprolol fumarate by application of hydrophilic interaction liquid chromatography. in Arhiv za farmaciju
Savez farmaceutskih udruženja Srbije, Beograd., 64(3), 230-246.
https://doi.org/10.5937/arhfarm1403230K
Kasagić-Vujanović I, Jančić-Stojanović B, Ivanović D. Study of forced degradation of amlodipine besylate and bisoprolol fumarate by application of hydrophilic interaction liquid chromatography. in Arhiv za farmaciju. 2014;64(3):230-246.
doi:10.5937/arhfarm1403230K .
Kasagić-Vujanović, Irena, Jančić-Stojanović, Biljana, Ivanović, Darko, "Study of forced degradation of amlodipine besylate and bisoprolol fumarate by application of hydrophilic interaction liquid chromatography" in Arhiv za farmaciju, 64, no. 3 (2014):230-246,
https://doi.org/10.5937/arhfarm1403230K . .
1
3

Comparison of Full Factorial Design, Central Composite Design, and Box-Behnken Design in Chromatographic Method Development for the Determination of Fluconazole and Its Impurities

Rakić, Tijana; Kasagić-Vujanović, Irena; Jovanović, Marko; Jančić-Stojanović, Biljana; Ivanović, Darko

(Taylor & Francis Inc, Philadelphia, 2014)

TY  - JOUR
AU  - Rakić, Tijana
AU  - Kasagić-Vujanović, Irena
AU  - Jovanović, Marko
AU  - Jančić-Stojanović, Biljana
AU  - Ivanović, Darko
PY  - 2014
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2223
AB  - This paper presents the development and optimization of a liquid chromatographic method for the determination of fluconazole and its impurities by experimental design methodology. Four experimental design types were applied: two-level full factorial design, central composite design, Box-Behnken design, and three-level full factorial design. The advantages and drawbacks of each design are described and detailed statistical evaluation of mathematical models was performed. The central composite design and three-level full factorial design created significantly better models comparing to the other methods. As the central composite design requires a smaller number of experiments, its models were used for theoretical examination of experimental space. Multiobjective optimization aiming to achieve maximal separation of all investigated substances and minimal analysis duration was performed by a grid point search. The defined optimal separation was achieved on a C-18 (125mmx4mm, 5 mu m particle size) column with a mobile phase consisting of acetonitrile and water (5mM ammonium formate) (15:85, v/v); a column temperature of 25 degrees C; a flow rate of 1.2mLmin(-1); and a detection wavelength of 260nm.
PB  - Taylor & Francis Inc, Philadelphia
T2  - Analytical Letters
T1  - Comparison of Full Factorial Design, Central Composite Design, and Box-Behnken Design in Chromatographic Method Development for the Determination of Fluconazole and Its Impurities
VL  - 47
IS  - 8
SP  - 1334
EP  - 1347
DO  - 10.1080/00032719.2013.867503
ER  - 
@article{
author = "Rakić, Tijana and Kasagić-Vujanović, Irena and Jovanović, Marko and Jančić-Stojanović, Biljana and Ivanović, Darko",
year = "2014",
abstract = "This paper presents the development and optimization of a liquid chromatographic method for the determination of fluconazole and its impurities by experimental design methodology. Four experimental design types were applied: two-level full factorial design, central composite design, Box-Behnken design, and three-level full factorial design. The advantages and drawbacks of each design are described and detailed statistical evaluation of mathematical models was performed. The central composite design and three-level full factorial design created significantly better models comparing to the other methods. As the central composite design requires a smaller number of experiments, its models were used for theoretical examination of experimental space. Multiobjective optimization aiming to achieve maximal separation of all investigated substances and minimal analysis duration was performed by a grid point search. The defined optimal separation was achieved on a C-18 (125mmx4mm, 5 mu m particle size) column with a mobile phase consisting of acetonitrile and water (5mM ammonium formate) (15:85, v/v); a column temperature of 25 degrees C; a flow rate of 1.2mLmin(-1); and a detection wavelength of 260nm.",
publisher = "Taylor & Francis Inc, Philadelphia",
journal = "Analytical Letters",
title = "Comparison of Full Factorial Design, Central Composite Design, and Box-Behnken Design in Chromatographic Method Development for the Determination of Fluconazole and Its Impurities",
volume = "47",
number = "8",
pages = "1334-1347",
doi = "10.1080/00032719.2013.867503"
}
Rakić, T., Kasagić-Vujanović, I., Jovanović, M., Jančić-Stojanović, B.,& Ivanović, D.. (2014). Comparison of Full Factorial Design, Central Composite Design, and Box-Behnken Design in Chromatographic Method Development for the Determination of Fluconazole and Its Impurities. in Analytical Letters
Taylor & Francis Inc, Philadelphia., 47(8), 1334-1347.
https://doi.org/10.1080/00032719.2013.867503
Rakić T, Kasagić-Vujanović I, Jovanović M, Jančić-Stojanović B, Ivanović D. Comparison of Full Factorial Design, Central Composite Design, and Box-Behnken Design in Chromatographic Method Development for the Determination of Fluconazole and Its Impurities. in Analytical Letters. 2014;47(8):1334-1347.
doi:10.1080/00032719.2013.867503 .
Rakić, Tijana, Kasagić-Vujanović, Irena, Jovanović, Marko, Jančić-Stojanović, Biljana, Ivanović, Darko, "Comparison of Full Factorial Design, Central Composite Design, and Box-Behnken Design in Chromatographic Method Development for the Determination of Fluconazole and Its Impurities" in Analytical Letters, 47, no. 8 (2014):1334-1347,
https://doi.org/10.1080/00032719.2013.867503 . .
1
145
85
157

Retention mechanism assessment and method development for the analysis of iohexol and its related compounds in hydrophilic interaction liquid chromatography

Jovanović, Marko; Rakić, Tijana; Jančić-Stojanović, Biljana; Ivanović, Darko; Medenica, Mirjana

(Springer Heidelberg, Heidelberg, 2014)

TY  - JOUR
AU  - Jovanović, Marko
AU  - Rakić, Tijana
AU  - Jančić-Stojanović, Biljana
AU  - Ivanović, Darko
AU  - Medenica, Mirjana
PY  - 2014
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2191
AB  - Hydrophilic interaction liquid chromatography (HILIC) has emerged in recent years as a valuable alternative to reversed-phase liquid chromatography in the analysis of polar compounds. Research in HILIC is divided into two directions: the assessment of the retention mechanism and retention behavior, and the development of HILIC methods. In this work, four polar neutral analytes (iohexol and its related compounds A, B, and C) were analyzed on two silica and two diol columns in HILIC mode with the aim to investigate thoroughly the retention mechanisms and retention behavior of polar neutral compounds on these four columns. The adsorption and partition contribution to the overall HILIC retention mechanism was investigated by fitting the retention data to linear (adsorption and partition) and nonlinear (mixed-retention and quadratic) theoretical models. On the other hand, the establishment of empirical second-order polynomial retention models on the basis of D-optimal design made possible the estimation of the simultaneous influence of several mobile-phase-related factors. Furthermore, these models were also used as the basis for the application of indirect modeling of the selectivity factor and a grid point search approach in order to achieve the optimal separation of analytes. After the optimization goals had been set, the grids were searched and the optimal conditions were identified. Finally, the optimized method was subjected to validation.
PB  - Springer Heidelberg, Heidelberg
T2  - Analytical and Bioanalytical Chemistry
T1  - Retention mechanism assessment and method development for the analysis of iohexol and its related compounds in hydrophilic interaction liquid chromatography
VL  - 406
IS  - 17
SP  - 4217
EP  - 4232
DO  - 10.1007/s00216-014-7808-6
ER  - 
@article{
author = "Jovanović, Marko and Rakić, Tijana and Jančić-Stojanović, Biljana and Ivanović, Darko and Medenica, Mirjana",
year = "2014",
abstract = "Hydrophilic interaction liquid chromatography (HILIC) has emerged in recent years as a valuable alternative to reversed-phase liquid chromatography in the analysis of polar compounds. Research in HILIC is divided into two directions: the assessment of the retention mechanism and retention behavior, and the development of HILIC methods. In this work, four polar neutral analytes (iohexol and its related compounds A, B, and C) were analyzed on two silica and two diol columns in HILIC mode with the aim to investigate thoroughly the retention mechanisms and retention behavior of polar neutral compounds on these four columns. The adsorption and partition contribution to the overall HILIC retention mechanism was investigated by fitting the retention data to linear (adsorption and partition) and nonlinear (mixed-retention and quadratic) theoretical models. On the other hand, the establishment of empirical second-order polynomial retention models on the basis of D-optimal design made possible the estimation of the simultaneous influence of several mobile-phase-related factors. Furthermore, these models were also used as the basis for the application of indirect modeling of the selectivity factor and a grid point search approach in order to achieve the optimal separation of analytes. After the optimization goals had been set, the grids were searched and the optimal conditions were identified. Finally, the optimized method was subjected to validation.",
publisher = "Springer Heidelberg, Heidelberg",
journal = "Analytical and Bioanalytical Chemistry",
title = "Retention mechanism assessment and method development for the analysis of iohexol and its related compounds in hydrophilic interaction liquid chromatography",
volume = "406",
number = "17",
pages = "4217-4232",
doi = "10.1007/s00216-014-7808-6"
}
Jovanović, M., Rakić, T., Jančić-Stojanović, B., Ivanović, D.,& Medenica, M.. (2014). Retention mechanism assessment and method development for the analysis of iohexol and its related compounds in hydrophilic interaction liquid chromatography. in Analytical and Bioanalytical Chemistry
Springer Heidelberg, Heidelberg., 406(17), 4217-4232.
https://doi.org/10.1007/s00216-014-7808-6
Jovanović M, Rakić T, Jančić-Stojanović B, Ivanović D, Medenica M. Retention mechanism assessment and method development for the analysis of iohexol and its related compounds in hydrophilic interaction liquid chromatography. in Analytical and Bioanalytical Chemistry. 2014;406(17):4217-4232.
doi:10.1007/s00216-014-7808-6 .
Jovanović, Marko, Rakić, Tijana, Jančić-Stojanović, Biljana, Ivanović, Darko, Medenica, Mirjana, "Retention mechanism assessment and method development for the analysis of iohexol and its related compounds in hydrophilic interaction liquid chromatography" in Analytical and Bioanalytical Chemistry, 406, no. 17 (2014):4217-4232,
https://doi.org/10.1007/s00216-014-7808-6 . .
7
7
6

Sports pharmacy: Pharmacists role in doping in sport

Ivanović, Darko; Stojanović, Biljana

(Savez farmaceutskih udruženja Srbije, Beograd, 2013)

TY  - JOUR
AU  - Ivanović, Darko
AU  - Stojanović, Biljana
PY  - 2013
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2055
AB  - In this paper, the role and importance of pharmacists in prevention of doping in sports is presented. Integrating all the competencies of a pharmacist into Sports pharmacy all the segments that emphasize the position and significance of pharmacists are presented. Regarding this discipline pharmacists assume the following responsibilities: advisory and education in doping prevention, work in laboratories for doping control, designing of a dietary regimen, drug application, drug supply and the analysis of drugs' influence on biochemical and hematological parameters as well. As a matter of fact, pharmacist should be an integral part of the team responsible for proper usage of drugs and dietary supplements not only in professional, but also in amateur sports. Acknowledging all the worldwide experience, the ways in which the pharmacists can take part in Sports pharmacy are also addressed in this paper. Regarding the fact that this discipline demands multidisciplinary approach, it is rather clear that experts from different areas of pharmacy should be included in pharmacists' education, thereby confirming the significance of Sports pharmacy.
AB  - U ovom radu prikazani su uloga i značaj farmaceuta u borbi protiv dopinga u sportu. Objedinjujući uloge farmaceuta u Sportsku farmaciju, prikazani su različiti segmenti u kojima se jasno naglašava koje je mesto i značaj farmaceuta. U ovoj disciplini farmaceut ima sledeće uloge: savetodavnu i edukativnu u prevenciji dopinga, rad u kontrolnim laboratorijama, zatim pravilno dizajniranje dijete, praćenje primene lekova, snabdevanje lekovima, kao i praćenje i analiziranje uticaja lekova na biohemijske i hematološke parametre. U svakom slučaju farmaceut treba da bude sastavni deo tima koji je odgovoran za pravilnu upotrebu lekova i dijetetskih suplemenata u sportu, bez obzira da li se radi o profesionalnim sportistima ili o sportistima amaterima. U radu je takođe prikazano na koji način se farmaceuti mogu uključiti u sportsku farmaciju, uzimajući u obzir iskustva koja postoje širom sveta. S obzirom na multidisciplinarnost koja je ovde posebno naglašena, jasno je da edukacija ima poseban značaj jer podrazumeva angažovanje stručnjaka iz različitih oblasti farmacije čime se i dodatno potvrđuje značaj Sportske farmacije.
PB  - Savez farmaceutskih udruženja Srbije, Beograd
T2  - Arhiv za farmaciju
T1  - Sports pharmacy: Pharmacists role in doping in sport
T1  - Sportska farmacija - uloga farmaceuta u borbi protiv dopinga u sportu
VL  - 63
IS  - 6
SP  - 528
EP  - 540
UR  - https://hdl.handle.net/21.15107/rcub_farfar_2055
ER  - 
@article{
author = "Ivanović, Darko and Stojanović, Biljana",
year = "2013",
abstract = "In this paper, the role and importance of pharmacists in prevention of doping in sports is presented. Integrating all the competencies of a pharmacist into Sports pharmacy all the segments that emphasize the position and significance of pharmacists are presented. Regarding this discipline pharmacists assume the following responsibilities: advisory and education in doping prevention, work in laboratories for doping control, designing of a dietary regimen, drug application, drug supply and the analysis of drugs' influence on biochemical and hematological parameters as well. As a matter of fact, pharmacist should be an integral part of the team responsible for proper usage of drugs and dietary supplements not only in professional, but also in amateur sports. Acknowledging all the worldwide experience, the ways in which the pharmacists can take part in Sports pharmacy are also addressed in this paper. Regarding the fact that this discipline demands multidisciplinary approach, it is rather clear that experts from different areas of pharmacy should be included in pharmacists' education, thereby confirming the significance of Sports pharmacy., U ovom radu prikazani su uloga i značaj farmaceuta u borbi protiv dopinga u sportu. Objedinjujući uloge farmaceuta u Sportsku farmaciju, prikazani su različiti segmenti u kojima se jasno naglašava koje je mesto i značaj farmaceuta. U ovoj disciplini farmaceut ima sledeće uloge: savetodavnu i edukativnu u prevenciji dopinga, rad u kontrolnim laboratorijama, zatim pravilno dizajniranje dijete, praćenje primene lekova, snabdevanje lekovima, kao i praćenje i analiziranje uticaja lekova na biohemijske i hematološke parametre. U svakom slučaju farmaceut treba da bude sastavni deo tima koji je odgovoran za pravilnu upotrebu lekova i dijetetskih suplemenata u sportu, bez obzira da li se radi o profesionalnim sportistima ili o sportistima amaterima. U radu je takođe prikazano na koji način se farmaceuti mogu uključiti u sportsku farmaciju, uzimajući u obzir iskustva koja postoje širom sveta. S obzirom na multidisciplinarnost koja je ovde posebno naglašena, jasno je da edukacija ima poseban značaj jer podrazumeva angažovanje stručnjaka iz različitih oblasti farmacije čime se i dodatno potvrđuje značaj Sportske farmacije.",
publisher = "Savez farmaceutskih udruženja Srbije, Beograd",
journal = "Arhiv za farmaciju",
title = "Sports pharmacy: Pharmacists role in doping in sport, Sportska farmacija - uloga farmaceuta u borbi protiv dopinga u sportu",
volume = "63",
number = "6",
pages = "528-540",
url = "https://hdl.handle.net/21.15107/rcub_farfar_2055"
}
Ivanović, D.,& Stojanović, B.. (2013). Sports pharmacy: Pharmacists role in doping in sport. in Arhiv za farmaciju
Savez farmaceutskih udruženja Srbije, Beograd., 63(6), 528-540.
https://hdl.handle.net/21.15107/rcub_farfar_2055
Ivanović D, Stojanović B. Sports pharmacy: Pharmacists role in doping in sport. in Arhiv za farmaciju. 2013;63(6):528-540.
https://hdl.handle.net/21.15107/rcub_farfar_2055 .
Ivanović, Darko, Stojanović, Biljana, "Sports pharmacy: Pharmacists role in doping in sport" in Arhiv za farmaciju, 63, no. 6 (2013):528-540,
https://hdl.handle.net/21.15107/rcub_farfar_2055 .

Evaluation of Seven Chromatographic Response Functions on Simulated and Experimentally Obtained Chromatograms in Hydrophilic Interaction Liquid Chromatography System

Rakić, Tijana; Jančić-Stojanović, Biljana; Jovanović, Marko; Malenović, Anđelija; Ivanović, Darko; Medenica, Mirjana

(Taylor & Francis Inc, Philadelphia, 2013)

TY  - JOUR
AU  - Rakić, Tijana
AU  - Jančić-Stojanović, Biljana
AU  - Jovanović, Marko
AU  - Malenović, Anđelija
AU  - Ivanović, Darko
AU  - Medenica, Mirjana
PY  - 2013
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/3419
AB  - This paper investigates the ability of seven chromatographic response functions to measure the quality of chromatograms obtained in hydrophilic interaction liquid chromatography (HILIC). First, the functions were tested on a set of simulated chromatograms and differences in their mathematical design were discussed. Second, the functions were evaluated on the experimentally obtained chromatograms in HILIC analysis of model mixture consisted of beta agonists and antagonists. The ranking of chromatograms obtained by different functions was significantly different, implying that the accuracy of the optimization procedure is strongly dependent on the function that was selected as an output. Investigation of potential drawbacks of each function was conducted and general recommendations concerning the use of chromatographic response functions in optimization strategies are proposed.
PB  - Taylor & Francis Inc, Philadelphia
T2  - Analytical Letters
T1  - Evaluation of Seven Chromatographic Response Functions on Simulated and Experimentally Obtained Chromatograms in Hydrophilic Interaction Liquid Chromatography System
VL  - 46
IS  - 8
SP  - 1198
EP  - 1212
DO  - 10.1080/00032719.2012.755689
ER  - 
@article{
author = "Rakić, Tijana and Jančić-Stojanović, Biljana and Jovanović, Marko and Malenović, Anđelija and Ivanović, Darko and Medenica, Mirjana",
year = "2013",
abstract = "This paper investigates the ability of seven chromatographic response functions to measure the quality of chromatograms obtained in hydrophilic interaction liquid chromatography (HILIC). First, the functions were tested on a set of simulated chromatograms and differences in their mathematical design were discussed. Second, the functions were evaluated on the experimentally obtained chromatograms in HILIC analysis of model mixture consisted of beta agonists and antagonists. The ranking of chromatograms obtained by different functions was significantly different, implying that the accuracy of the optimization procedure is strongly dependent on the function that was selected as an output. Investigation of potential drawbacks of each function was conducted and general recommendations concerning the use of chromatographic response functions in optimization strategies are proposed.",
publisher = "Taylor & Francis Inc, Philadelphia",
journal = "Analytical Letters",
title = "Evaluation of Seven Chromatographic Response Functions on Simulated and Experimentally Obtained Chromatograms in Hydrophilic Interaction Liquid Chromatography System",
volume = "46",
number = "8",
pages = "1198-1212",
doi = "10.1080/00032719.2012.755689"
}
Rakić, T., Jančić-Stojanović, B., Jovanović, M., Malenović, A., Ivanović, D.,& Medenica, M.. (2013). Evaluation of Seven Chromatographic Response Functions on Simulated and Experimentally Obtained Chromatograms in Hydrophilic Interaction Liquid Chromatography System. in Analytical Letters
Taylor & Francis Inc, Philadelphia., 46(8), 1198-1212.
https://doi.org/10.1080/00032719.2012.755689
Rakić T, Jančić-Stojanović B, Jovanović M, Malenović A, Ivanović D, Medenica M. Evaluation of Seven Chromatographic Response Functions on Simulated and Experimentally Obtained Chromatograms in Hydrophilic Interaction Liquid Chromatography System. in Analytical Letters. 2013;46(8):1198-1212.
doi:10.1080/00032719.2012.755689 .
Rakić, Tijana, Jančić-Stojanović, Biljana, Jovanović, Marko, Malenović, Anđelija, Ivanović, Darko, Medenica, Mirjana, "Evaluation of Seven Chromatographic Response Functions on Simulated and Experimentally Obtained Chromatograms in Hydrophilic Interaction Liquid Chromatography System" in Analytical Letters, 46, no. 8 (2013):1198-1212,
https://doi.org/10.1080/00032719.2012.755689 . .
3
3
3

Chemometrically assissted optimization and validation of RP-HPLC method for the analysis of itraconazole and its impurities

Kasagić-Vujanović, Irena; Malenović, Anđelija; Jovanović, Marko; Rakić, Tijana; Jančić-Stojanović, Biljana; Ivanović, Darko

(Hrvatsko Farmaceutsko Drustov (HFD)-Croation Pharmaceutical Soc, Zagreb, 2013)

TY  - JOUR
AU  - Kasagić-Vujanović, Irena
AU  - Malenović, Anđelija
AU  - Jovanović, Marko
AU  - Rakić, Tijana
AU  - Jančić-Stojanović, Biljana
AU  - Ivanović, Darko
PY  - 2013
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/1920
AB  - This paper presents the chemometrically assisted optimization and validation of the RP-HPLC method intended for the quantitative analysis of itraconazole and its impurities in pharmaceutical dosage forms. To reach the desired chromatographic resolution with a limited number of experiments in a minimum amount of time, Box-Behnken design was used to simultaneously optimize some important chromatographic parameters, such as the acetonitrile content in the mobile phase, pH of the aqueous phase and the column temperature. Separation between itraconazole and impurity F was identified as critical and selected as a response during the optimization. The set optimal mobile phase composition was acetonitrile/water pH 2.5 adjusted with o-phosphoric acid (50:50, V/V). Separations were performed on a Zorbax Eclipse XDB-C18, 4.6 x 150 mm, 5 mu m particle size column with the flow rate 1 mL min(-1), column temperature set at 30 degrees C and UV detection at 256 nm. The established method was then subjected to method validation and the required validation parameters were tested. For the robustness evaluation, fractional factorial 2(4-1) design was utilized and factors that might significantly affect the system performance were defined. As other validation parameters were also found to be suitable, the possibility to apply the proposed method for the determination of itraconazole, its impurities B and F in any laboratory under different circumstances has been proven.
PB  - Hrvatsko Farmaceutsko Drustov (HFD)-Croation Pharmaceutical Soc, Zagreb
T2  - Acta Pharmaceutica
T1  - Chemometrically assissted optimization and validation of RP-HPLC method for the analysis of itraconazole and its impurities
VL  - 63
IS  - 2
SP  - 159
EP  - 173
DO  - 10.2478/acph-2013-0015
ER  - 
@article{
author = "Kasagić-Vujanović, Irena and Malenović, Anđelija and Jovanović, Marko and Rakić, Tijana and Jančić-Stojanović, Biljana and Ivanović, Darko",
year = "2013",
abstract = "This paper presents the chemometrically assisted optimization and validation of the RP-HPLC method intended for the quantitative analysis of itraconazole and its impurities in pharmaceutical dosage forms. To reach the desired chromatographic resolution with a limited number of experiments in a minimum amount of time, Box-Behnken design was used to simultaneously optimize some important chromatographic parameters, such as the acetonitrile content in the mobile phase, pH of the aqueous phase and the column temperature. Separation between itraconazole and impurity F was identified as critical and selected as a response during the optimization. The set optimal mobile phase composition was acetonitrile/water pH 2.5 adjusted with o-phosphoric acid (50:50, V/V). Separations were performed on a Zorbax Eclipse XDB-C18, 4.6 x 150 mm, 5 mu m particle size column with the flow rate 1 mL min(-1), column temperature set at 30 degrees C and UV detection at 256 nm. The established method was then subjected to method validation and the required validation parameters were tested. For the robustness evaluation, fractional factorial 2(4-1) design was utilized and factors that might significantly affect the system performance were defined. As other validation parameters were also found to be suitable, the possibility to apply the proposed method for the determination of itraconazole, its impurities B and F in any laboratory under different circumstances has been proven.",
publisher = "Hrvatsko Farmaceutsko Drustov (HFD)-Croation Pharmaceutical Soc, Zagreb",
journal = "Acta Pharmaceutica",
title = "Chemometrically assissted optimization and validation of RP-HPLC method for the analysis of itraconazole and its impurities",
volume = "63",
number = "2",
pages = "159-173",
doi = "10.2478/acph-2013-0015"
}
Kasagić-Vujanović, I., Malenović, A., Jovanović, M., Rakić, T., Jančić-Stojanović, B.,& Ivanović, D.. (2013). Chemometrically assissted optimization and validation of RP-HPLC method for the analysis of itraconazole and its impurities. in Acta Pharmaceutica
Hrvatsko Farmaceutsko Drustov (HFD)-Croation Pharmaceutical Soc, Zagreb., 63(2), 159-173.
https://doi.org/10.2478/acph-2013-0015
Kasagić-Vujanović I, Malenović A, Jovanović M, Rakić T, Jančić-Stojanović B, Ivanović D. Chemometrically assissted optimization and validation of RP-HPLC method for the analysis of itraconazole and its impurities. in Acta Pharmaceutica. 2013;63(2):159-173.
doi:10.2478/acph-2013-0015 .
Kasagić-Vujanović, Irena, Malenović, Anđelija, Jovanović, Marko, Rakić, Tijana, Jančić-Stojanović, Biljana, Ivanović, Darko, "Chemometrically assissted optimization and validation of RP-HPLC method for the analysis of itraconazole and its impurities" in Acta Pharmaceutica, 63, no. 2 (2013):159-173,
https://doi.org/10.2478/acph-2013-0015 . .
13
11
16

Five different columns in the analysis of basic drugs in hydrophilic interaction liquid chromatography

Jovanović, Marko; Jančić-Stojanović, Biljana; Rakić, Tijana; Malenović, Anđelija; Ivanović, Darko; Medenica, Mirjana

(Versita, Warsaw, 2013)

TY  - JOUR
AU  - Jovanović, Marko
AU  - Jančić-Stojanović, Biljana
AU  - Rakić, Tijana
AU  - Malenović, Anđelija
AU  - Ivanović, Darko
AU  - Medenica, Mirjana
PY  - 2013
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2001
AB  - Five different columns (two silica, two cyanopropyl and one diol) were investigated in hydrophilic interaction liquid chromatography (HILIC). For the assessment of columns behavior in HILIC mode, six basic drugs (lamotrigine, thioridazine, clozapine, chlorpheniramine, pheniramine and sulpiride) were chosen. The assessment of the influence of the concentration of organic modifier on analytes' retention on each column was provided by fitting the retention data into theoretical models. Utilizing the statistical analysis, the selection of the model that provides better prediction of the retention behavior was enabled. Dual RP-HILIC mechanism was suggested on cyanopropyl and diol columns, therefore the transition points between the two mechanisms on these columns were calculated. Furthermore, in order to investigate the impact of three factors simultaneously on the retention behavior of the analyzed substances on Betasil Silica column, chemometrically-aided empirical models were built. The experiments were conducted according to the matrix of Box-Behnken design and on the basis of the retention data, six quadratic models were obtained and their adequacy was confirmed using ANOVA test. The obtained coefficients of quadratic models enabled the elucidation of both single factor and factor interactions influence. This was also graphically presented in 3D response surface plots.
PB  - Versita, Warsaw
T2  - Central European Journal of Chemistry
T1  - Five different columns in the analysis of basic drugs in hydrophilic interaction liquid chromatography
VL  - 11
IS  - 7
SP  - 1150
EP  - 1162
DO  - 10.2478/s11532-013-0245-0
ER  - 
@article{
author = "Jovanović, Marko and Jančić-Stojanović, Biljana and Rakić, Tijana and Malenović, Anđelija and Ivanović, Darko and Medenica, Mirjana",
year = "2013",
abstract = "Five different columns (two silica, two cyanopropyl and one diol) were investigated in hydrophilic interaction liquid chromatography (HILIC). For the assessment of columns behavior in HILIC mode, six basic drugs (lamotrigine, thioridazine, clozapine, chlorpheniramine, pheniramine and sulpiride) were chosen. The assessment of the influence of the concentration of organic modifier on analytes' retention on each column was provided by fitting the retention data into theoretical models. Utilizing the statistical analysis, the selection of the model that provides better prediction of the retention behavior was enabled. Dual RP-HILIC mechanism was suggested on cyanopropyl and diol columns, therefore the transition points between the two mechanisms on these columns were calculated. Furthermore, in order to investigate the impact of three factors simultaneously on the retention behavior of the analyzed substances on Betasil Silica column, chemometrically-aided empirical models were built. The experiments were conducted according to the matrix of Box-Behnken design and on the basis of the retention data, six quadratic models were obtained and their adequacy was confirmed using ANOVA test. The obtained coefficients of quadratic models enabled the elucidation of both single factor and factor interactions influence. This was also graphically presented in 3D response surface plots.",
publisher = "Versita, Warsaw",
journal = "Central European Journal of Chemistry",
title = "Five different columns in the analysis of basic drugs in hydrophilic interaction liquid chromatography",
volume = "11",
number = "7",
pages = "1150-1162",
doi = "10.2478/s11532-013-0245-0"
}
Jovanović, M., Jančić-Stojanović, B., Rakić, T., Malenović, A., Ivanović, D.,& Medenica, M.. (2013). Five different columns in the analysis of basic drugs in hydrophilic interaction liquid chromatography. in Central European Journal of Chemistry
Versita, Warsaw., 11(7), 1150-1162.
https://doi.org/10.2478/s11532-013-0245-0
Jovanović M, Jančić-Stojanović B, Rakić T, Malenović A, Ivanović D, Medenica M. Five different columns in the analysis of basic drugs in hydrophilic interaction liquid chromatography. in Central European Journal of Chemistry. 2013;11(7):1150-1162.
doi:10.2478/s11532-013-0245-0 .
Jovanović, Marko, Jančić-Stojanović, Biljana, Rakić, Tijana, Malenović, Anđelija, Ivanović, Darko, Medenica, Mirjana, "Five different columns in the analysis of basic drugs in hydrophilic interaction liquid chromatography" in Central European Journal of Chemistry, 11, no. 7 (2013):1150-1162,
https://doi.org/10.2478/s11532-013-0245-0 . .
11
10
11

Evaluation of Seven Chromatographic Response Functions on Simulated and Experimentally Obtained Chromatograms in Hydrophilic Interaction Liquid Chromatography System

Rakić, Tijana; Jančić-Stojanović, Biljana; Jovanović, Marko; Malenović, Anđelija; Ivanović, Darko; Medenica, Mirjana

(Taylor & Francis Inc, Philadelphia, 2013)

TY  - JOUR
AU  - Rakić, Tijana
AU  - Jančić-Stojanović, Biljana
AU  - Jovanović, Marko
AU  - Malenović, Anđelija
AU  - Ivanović, Darko
AU  - Medenica, Mirjana
PY  - 2013
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2003
AB  - This paper investigates the ability of seven chromatographic response functions to measure the quality of chromatograms obtained in hydrophilic interaction liquid chromatography (HILIC). First, the functions were tested on a set of simulated chromatograms and differences in their mathematical design were discussed. Second, the functions were evaluated on the experimentally obtained chromatograms in HILIC analysis of model mixture consisted of beta agonists and antagonists. The ranking of chromatograms obtained by different functions was significantly different, implying that the accuracy of the optimization procedure is strongly dependent on the function that was selected as an output. Investigation of potential drawbacks of each function was conducted and general recommendations concerning the use of chromatographic response functions in optimization strategies are proposed.
PB  - Taylor & Francis Inc, Philadelphia
T2  - Analytical Letters
T1  - Evaluation of Seven Chromatographic Response Functions on Simulated and Experimentally Obtained Chromatograms in Hydrophilic Interaction Liquid Chromatography System
VL  - 46
IS  - 8
SP  - 1198
EP  - 1212
DO  - 10.1080/00032719.2012.755689
ER  - 
@article{
author = "Rakić, Tijana and Jančić-Stojanović, Biljana and Jovanović, Marko and Malenović, Anđelija and Ivanović, Darko and Medenica, Mirjana",
year = "2013",
abstract = "This paper investigates the ability of seven chromatographic response functions to measure the quality of chromatograms obtained in hydrophilic interaction liquid chromatography (HILIC). First, the functions were tested on a set of simulated chromatograms and differences in their mathematical design were discussed. Second, the functions were evaluated on the experimentally obtained chromatograms in HILIC analysis of model mixture consisted of beta agonists and antagonists. The ranking of chromatograms obtained by different functions was significantly different, implying that the accuracy of the optimization procedure is strongly dependent on the function that was selected as an output. Investigation of potential drawbacks of each function was conducted and general recommendations concerning the use of chromatographic response functions in optimization strategies are proposed.",
publisher = "Taylor & Francis Inc, Philadelphia",
journal = "Analytical Letters",
title = "Evaluation of Seven Chromatographic Response Functions on Simulated and Experimentally Obtained Chromatograms in Hydrophilic Interaction Liquid Chromatography System",
volume = "46",
number = "8",
pages = "1198-1212",
doi = "10.1080/00032719.2012.755689"
}
Rakić, T., Jančić-Stojanović, B., Jovanović, M., Malenović, A., Ivanović, D.,& Medenica, M.. (2013). Evaluation of Seven Chromatographic Response Functions on Simulated and Experimentally Obtained Chromatograms in Hydrophilic Interaction Liquid Chromatography System. in Analytical Letters
Taylor & Francis Inc, Philadelphia., 46(8), 1198-1212.
https://doi.org/10.1080/00032719.2012.755689
Rakić T, Jančić-Stojanović B, Jovanović M, Malenović A, Ivanović D, Medenica M. Evaluation of Seven Chromatographic Response Functions on Simulated and Experimentally Obtained Chromatograms in Hydrophilic Interaction Liquid Chromatography System. in Analytical Letters. 2013;46(8):1198-1212.
doi:10.1080/00032719.2012.755689 .
Rakić, Tijana, Jančić-Stojanović, Biljana, Jovanović, Marko, Malenović, Anđelija, Ivanović, Darko, Medenica, Mirjana, "Evaluation of Seven Chromatographic Response Functions on Simulated and Experimentally Obtained Chromatograms in Hydrophilic Interaction Liquid Chromatography System" in Analytical Letters, 46, no. 8 (2013):1198-1212,
https://doi.org/10.1080/00032719.2012.755689 . .
3
3
3

Stepwise optimization approach for improving LC-MS/MS analysis of zwitterionic antiepileptic drugs with implementation of experimental design

Kostić, Nada; Dotsikas, Yannis; Malenović, Anđelija; Jančić-Stojanović, Biljana; Rakić, Tijana; Ivanović, Darko; Medenica, Mirjana

(Wiley-Blackwell, Hoboken, 2013)

TY  - JOUR
AU  - Kostić, Nada
AU  - Dotsikas, Yannis
AU  - Malenović, Anđelija
AU  - Jančić-Stojanović, Biljana
AU  - Rakić, Tijana
AU  - Ivanović, Darko
AU  - Medenica, Mirjana
PY  - 2013
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/1967
AB  - In this article, a step-by-step optimization procedure for improving analyte response with implementation of experimental design is described. Zwitterionic antiepileptics, namely vigabatrin, pregabalin and gabapentin, were chosen as model compounds to undergo chloroformate-mediated derivatization followed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) analysis. Application of a planned stepwise optimization procedure allowed responses of analytes, expressed as areas and signal-to-noise ratios, to be improved, enabling achievement of lower limit of detection values. Results from the current study demonstrate that optimization of parameters such as scan time, geometry of ion source, sheath and auxiliary gas pressure, capillary temperature, collision pressure and mobile phase composition can have a positive impact on sensitivity of LC-MS/MS methods. Optimization of LC and MS parameters led to a total increment of 53.9%, 83.3% and 95.7% in areas of derivatized vigabatrin, pregabalin and gabapentin, respectively, while for signal-to-noise values, an improvement of 140.0%, 93.6% and 124.0% was achieved, compared to autotune settings. After defining the final optimal conditions, a time-segmented method was validated for the determination of mentioned drugs in plasma. The method proved to be accurate and precise with excellent linearity for the tested concentration range (40.0ngml(-1)-10.0x10(3)ngml(-1)). Copyright
PB  - Wiley-Blackwell, Hoboken
T2  - Journal of Mass Spectrometry
T1  - Stepwise optimization approach for improving LC-MS/MS analysis of zwitterionic antiepileptic drugs with implementation of experimental design
VL  - 48
IS  - 7
SP  - 875
EP  - 884
DO  - 10.1002/jms.3236
ER  - 
@article{
author = "Kostić, Nada and Dotsikas, Yannis and Malenović, Anđelija and Jančić-Stojanović, Biljana and Rakić, Tijana and Ivanović, Darko and Medenica, Mirjana",
year = "2013",
abstract = "In this article, a step-by-step optimization procedure for improving analyte response with implementation of experimental design is described. Zwitterionic antiepileptics, namely vigabatrin, pregabalin and gabapentin, were chosen as model compounds to undergo chloroformate-mediated derivatization followed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) analysis. Application of a planned stepwise optimization procedure allowed responses of analytes, expressed as areas and signal-to-noise ratios, to be improved, enabling achievement of lower limit of detection values. Results from the current study demonstrate that optimization of parameters such as scan time, geometry of ion source, sheath and auxiliary gas pressure, capillary temperature, collision pressure and mobile phase composition can have a positive impact on sensitivity of LC-MS/MS methods. Optimization of LC and MS parameters led to a total increment of 53.9%, 83.3% and 95.7% in areas of derivatized vigabatrin, pregabalin and gabapentin, respectively, while for signal-to-noise values, an improvement of 140.0%, 93.6% and 124.0% was achieved, compared to autotune settings. After defining the final optimal conditions, a time-segmented method was validated for the determination of mentioned drugs in plasma. The method proved to be accurate and precise with excellent linearity for the tested concentration range (40.0ngml(-1)-10.0x10(3)ngml(-1)). Copyright",
publisher = "Wiley-Blackwell, Hoboken",
journal = "Journal of Mass Spectrometry",
title = "Stepwise optimization approach for improving LC-MS/MS analysis of zwitterionic antiepileptic drugs with implementation of experimental design",
volume = "48",
number = "7",
pages = "875-884",
doi = "10.1002/jms.3236"
}
Kostić, N., Dotsikas, Y., Malenović, A., Jančić-Stojanović, B., Rakić, T., Ivanović, D.,& Medenica, M.. (2013). Stepwise optimization approach for improving LC-MS/MS analysis of zwitterionic antiepileptic drugs with implementation of experimental design. in Journal of Mass Spectrometry
Wiley-Blackwell, Hoboken., 48(7), 875-884.
https://doi.org/10.1002/jms.3236
Kostić N, Dotsikas Y, Malenović A, Jančić-Stojanović B, Rakić T, Ivanović D, Medenica M. Stepwise optimization approach for improving LC-MS/MS analysis of zwitterionic antiepileptic drugs with implementation of experimental design. in Journal of Mass Spectrometry. 2013;48(7):875-884.
doi:10.1002/jms.3236 .
Kostić, Nada, Dotsikas, Yannis, Malenović, Anđelija, Jančić-Stojanović, Biljana, Rakić, Tijana, Ivanović, Darko, Medenica, Mirjana, "Stepwise optimization approach for improving LC-MS/MS analysis of zwitterionic antiepileptic drugs with implementation of experimental design" in Journal of Mass Spectrometry, 48, no. 7 (2013):875-884,
https://doi.org/10.1002/jms.3236 . .
1
20
19
20

Robustness testing of liquid chromatographic method for determination of itraconazole and its impurities applying fractional factorial design

Kasagić-Vujanović, Irena; Jovanović, Marko; Rakić, Tijana; Jančić-Stojanović, Biljana; Ivanović, Darko

(Savez farmaceutskih udruženja Srbije, Beograd, 2012)

TY  - JOUR
AU  - Kasagić-Vujanović, Irena
AU  - Jovanović, Marko
AU  - Rakić, Tijana
AU  - Jančić-Stojanović, Biljana
AU  - Ivanović, Darko
PY  - 2012
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/1815
AB  - Test of robustness is a part of the method validation and it is carried out in the end of the method development or in the beginning of the method validation. The purpose of robustness testing is to avoid problems in interlaboratory studies and to define parameters with the greatest impact on the method. The chosen factors are investigated within the range that slightly exceeds the expected variations when the method is transferred from one instrument/laboratory to another. The application of experimental design is recommended to perform robustness testing and two most often utilized - Plackett-Burman and fractional factorial design - are described. Furthermore, the manners of evaluation of factor significance, the methods for calculation of the range of insignificance for significant factors and the procedure for determination of system suitability test parameters are described. Such an approach of robustness testing was applied to the high performance liquid chromatographic method for determination of itraconazole and its impurities B and F. The robustness is tested by using fractional factorial design and 4 factors in 11 experiments were analyzed. After the application and the analysis of all the suggested steps for robustness, the impact of factors on the system responses was evaluated, insignificance ranges were defined and system suitability test limits for suggested method were determined.
AB  - Test robusnosti metode predstavlja deo validacije metode, a izvodi se na kraju razvoja metode ili na početku validacije. Testiranje robusnosti je uvedeno da bi se izbegli problemi u međulaboratorijskim ispitivanjima i da bi se definisali faktori koji imaju najveći uticaj na metodu. Izabrani faktori ispituju se u intervalu koji blago prevazilazi varijacije koje se očekuju kada se metoda prenosi sa jednog instrumenta/laboratorije na drugi. Za testiranje robusnosti korisno je primeniti eksperimentalni dizajn. U ovom radu opisana su dva najčešće korišćena, Plakett-Burman-ov i frakcioni faktorski dizajn. Takođe, opisani su i načini procene značajnosti faktora, zatim načini izračunavanja intervala neznačajnosti za značajne faktore, kao i postupak određivanja parametara za procenu pogodnosti sistema. Ovakav pristup procene robusnosti metode primenjen je na metodu tečne hromatografije za određivanje itrakonazola i njegovih nečistoća B i F. Robusnost je testirana primenom frakcionog faktorskog dizajna, a analizirana su četiri faktora kroz 11 eksperimenata. Sprovodeći i analizirajući sve predložene korake za robusnost procenjen je uticaj faktora na faktore rezolucije kao odgovore sistema, definisani su intervali neznačajnosti i određeni limiti za proveru pogodnosti sistema predložene metode.
PB  - Savez farmaceutskih udruženja Srbije, Beograd
T2  - Arhiv za farmaciju
T1  - Robustness testing of liquid chromatographic method for determination of itraconazole and its impurities applying fractional factorial design
T1  - Testiranje robusnosti metode tečne hromatografije za određivanje itrakonazola i njegovih nečistoća primenom frakcionog faktorskog dizajna
VL  - 62
IS  - 5
SP  - 475
EP  - 488
UR  - https://hdl.handle.net/21.15107/rcub_farfar_1815
ER  - 
@article{
author = "Kasagić-Vujanović, Irena and Jovanović, Marko and Rakić, Tijana and Jančić-Stojanović, Biljana and Ivanović, Darko",
year = "2012",
abstract = "Test of robustness is a part of the method validation and it is carried out in the end of the method development or in the beginning of the method validation. The purpose of robustness testing is to avoid problems in interlaboratory studies and to define parameters with the greatest impact on the method. The chosen factors are investigated within the range that slightly exceeds the expected variations when the method is transferred from one instrument/laboratory to another. The application of experimental design is recommended to perform robustness testing and two most often utilized - Plackett-Burman and fractional factorial design - are described. Furthermore, the manners of evaluation of factor significance, the methods for calculation of the range of insignificance for significant factors and the procedure for determination of system suitability test parameters are described. Such an approach of robustness testing was applied to the high performance liquid chromatographic method for determination of itraconazole and its impurities B and F. The robustness is tested by using fractional factorial design and 4 factors in 11 experiments were analyzed. After the application and the analysis of all the suggested steps for robustness, the impact of factors on the system responses was evaluated, insignificance ranges were defined and system suitability test limits for suggested method were determined., Test robusnosti metode predstavlja deo validacije metode, a izvodi se na kraju razvoja metode ili na početku validacije. Testiranje robusnosti je uvedeno da bi se izbegli problemi u međulaboratorijskim ispitivanjima i da bi se definisali faktori koji imaju najveći uticaj na metodu. Izabrani faktori ispituju se u intervalu koji blago prevazilazi varijacije koje se očekuju kada se metoda prenosi sa jednog instrumenta/laboratorije na drugi. Za testiranje robusnosti korisno je primeniti eksperimentalni dizajn. U ovom radu opisana su dva najčešće korišćena, Plakett-Burman-ov i frakcioni faktorski dizajn. Takođe, opisani su i načini procene značajnosti faktora, zatim načini izračunavanja intervala neznačajnosti za značajne faktore, kao i postupak određivanja parametara za procenu pogodnosti sistema. Ovakav pristup procene robusnosti metode primenjen je na metodu tečne hromatografije za određivanje itrakonazola i njegovih nečistoća B i F. Robusnost je testirana primenom frakcionog faktorskog dizajna, a analizirana su četiri faktora kroz 11 eksperimenata. Sprovodeći i analizirajući sve predložene korake za robusnost procenjen je uticaj faktora na faktore rezolucije kao odgovore sistema, definisani su intervali neznačajnosti i određeni limiti za proveru pogodnosti sistema predložene metode.",
publisher = "Savez farmaceutskih udruženja Srbije, Beograd",
journal = "Arhiv za farmaciju",
title = "Robustness testing of liquid chromatographic method for determination of itraconazole and its impurities applying fractional factorial design, Testiranje robusnosti metode tečne hromatografije za određivanje itrakonazola i njegovih nečistoća primenom frakcionog faktorskog dizajna",
volume = "62",
number = "5",
pages = "475-488",
url = "https://hdl.handle.net/21.15107/rcub_farfar_1815"
}
Kasagić-Vujanović, I., Jovanović, M., Rakić, T., Jančić-Stojanović, B.,& Ivanović, D.. (2012). Robustness testing of liquid chromatographic method for determination of itraconazole and its impurities applying fractional factorial design. in Arhiv za farmaciju
Savez farmaceutskih udruženja Srbije, Beograd., 62(5), 475-488.
https://hdl.handle.net/21.15107/rcub_farfar_1815
Kasagić-Vujanović I, Jovanović M, Rakić T, Jančić-Stojanović B, Ivanović D. Robustness testing of liquid chromatographic method for determination of itraconazole and its impurities applying fractional factorial design. in Arhiv za farmaciju. 2012;62(5):475-488.
https://hdl.handle.net/21.15107/rcub_farfar_1815 .
Kasagić-Vujanović, Irena, Jovanović, Marko, Rakić, Tijana, Jančić-Stojanović, Biljana, Ivanović, Darko, "Robustness testing of liquid chromatographic method for determination of itraconazole and its impurities applying fractional factorial design" in Arhiv za farmaciju, 62, no. 5 (2012):475-488,
https://hdl.handle.net/21.15107/rcub_farfar_1815 .
1

Physicochemical Factors Governing the Partition of Pramipexole and Its Five Impurities in Microemulsion Liquid Chromatographic Systems

Vemić, Ana; Malenović, Anđelija; Rakić, Tijana; Kostić, Nada M.; Jančić-Stojanović, Biljana; Ivanović, Darko; Medenica, Mirjana

(Soc Brasileira Quimica, Sao Paulo, 2012)

TY  - JOUR
AU  - Vemić, Ana
AU  - Malenović, Anđelija
AU  - Rakić, Tijana
AU  - Kostić, Nada M.
AU  - Jančić-Stojanović, Biljana
AU  - Ivanović, Darko
AU  - Medenica, Mirjana
PY  - 2012
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/1681
AB  - Microemulsions when used as mobile phases represent a very powerful chromatographic tool due to their polyphase structure. The aim of this study was to investigate the influence of the mobile phase composition and resulting microemulsion droplet's properties, as well as the stationary phase lipophilicity on the chromatographic behavior of pramipexole and its five impurities. Investigation was carried out according to the experimental plan defined by a full factorial design 2(4) with four central point replications. While the most affected by column characteristics was the last eluting, most lipophilic substance, the composition and characteristics of microemulsion droplets were equally important, so the partition system microemulsion droplets/stationary phase proved to be the most significant. Stationary phase lipophilicity did not affect the most hydrophilic component and only the partition system microemulsion droplets/bulk of the eluent impacted its behavior. For the separation of the critical pair, almost equal effects of the microemulsion droplets/stationary phase and bulk of the eluent/stationary phase partition systems were noted.
PB  - Soc Brasileira Quimica, Sao Paulo
T2  - Journal of the Brazilian Chemical Society
T1  - Physicochemical Factors Governing the Partition of Pramipexole and Its Five Impurities in Microemulsion Liquid Chromatographic Systems
VL  - 23
IS  - 11
SP  - 2084
EP  - 2092
UR  - https://hdl.handle.net/21.15107/rcub_farfar_1681
ER  - 
@article{
author = "Vemić, Ana and Malenović, Anđelija and Rakić, Tijana and Kostić, Nada M. and Jančić-Stojanović, Biljana and Ivanović, Darko and Medenica, Mirjana",
year = "2012",
abstract = "Microemulsions when used as mobile phases represent a very powerful chromatographic tool due to their polyphase structure. The aim of this study was to investigate the influence of the mobile phase composition and resulting microemulsion droplet's properties, as well as the stationary phase lipophilicity on the chromatographic behavior of pramipexole and its five impurities. Investigation was carried out according to the experimental plan defined by a full factorial design 2(4) with four central point replications. While the most affected by column characteristics was the last eluting, most lipophilic substance, the composition and characteristics of microemulsion droplets were equally important, so the partition system microemulsion droplets/stationary phase proved to be the most significant. Stationary phase lipophilicity did not affect the most hydrophilic component and only the partition system microemulsion droplets/bulk of the eluent impacted its behavior. For the separation of the critical pair, almost equal effects of the microemulsion droplets/stationary phase and bulk of the eluent/stationary phase partition systems were noted.",
publisher = "Soc Brasileira Quimica, Sao Paulo",
journal = "Journal of the Brazilian Chemical Society",
title = "Physicochemical Factors Governing the Partition of Pramipexole and Its Five Impurities in Microemulsion Liquid Chromatographic Systems",
volume = "23",
number = "11",
pages = "2084-2092",
url = "https://hdl.handle.net/21.15107/rcub_farfar_1681"
}
Vemić, A., Malenović, A., Rakić, T., Kostić, N. M., Jančić-Stojanović, B., Ivanović, D.,& Medenica, M.. (2012). Physicochemical Factors Governing the Partition of Pramipexole and Its Five Impurities in Microemulsion Liquid Chromatographic Systems. in Journal of the Brazilian Chemical Society
Soc Brasileira Quimica, Sao Paulo., 23(11), 2084-2092.
https://hdl.handle.net/21.15107/rcub_farfar_1681
Vemić A, Malenović A, Rakić T, Kostić NM, Jančić-Stojanović B, Ivanović D, Medenica M. Physicochemical Factors Governing the Partition of Pramipexole and Its Five Impurities in Microemulsion Liquid Chromatographic Systems. in Journal of the Brazilian Chemical Society. 2012;23(11):2084-2092.
https://hdl.handle.net/21.15107/rcub_farfar_1681 .
Vemić, Ana, Malenović, Anđelija, Rakić, Tijana, Kostić, Nada M., Jančić-Stojanović, Biljana, Ivanović, Darko, Medenica, Mirjana, "Physicochemical Factors Governing the Partition of Pramipexole and Its Five Impurities in Microemulsion Liquid Chromatographic Systems" in Journal of the Brazilian Chemical Society, 23, no. 11 (2012):2084-2092,
https://hdl.handle.net/21.15107/rcub_farfar_1681 .
5
6

Avoiding the False Negative Results in LC Method Robustness Testing by Modifications of the Algorithm of Dong and Dummy Factor Effects Approach

Rakić, Tijana; Malenović, Anđelija; Jančić-Stojanović, Biljana; Ivanović, Darko; Medenica, Mirjana

(Springer Heidelberg, Heidelberg, 2012)

TY  - JOUR
AU  - Rakić, Tijana
AU  - Malenović, Anđelija
AU  - Jančić-Stojanović, Biljana
AU  - Ivanović, Darko
AU  - Medenica, Mirjana
PY  - 2012
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/1758
AB  - The algorithm of Dong and error estimation based on a priori declared negligible effects (dummy factor effects approach) were evaluated for testing robustness, in case they provide contradictory results. Robustness of LC method for separation of ropinirole and its impurity was determined. Plackett-Burman design was applied to unravel the significant/influential factors. Four selected responses (retention factor of ropinirole and impurity, selectivity and resolution) were analyzed by the standard algorithm of Dong and dummy factor effects approach. The interpretation of the results for retention factor of ropinirole and resolution was inconclusive, since the two applied approaches identified different significant factors. The potential false negative or false positive results were avoided reanalyzing the results by the modified approaches. Modification of the dummy factor effects approach included omitting the large dummy effects values, and modification of the algorithm of Dong included calculating the margin of error values for all different number of factors included, and then selecting the lowest one to be the critical effect. The applied reanalysis allowed final important factor identification and non-significant intervals for significant effects calculation.
PB  - Springer Heidelberg, Heidelberg
T2  - Chromatographia
T1  - Avoiding the False Negative Results in LC Method Robustness Testing by Modifications of the Algorithm of Dong and Dummy Factor Effects Approach
VL  - 75
IS  - 7-8
SP  - 397
EP  - 401
DO  - 10.1007/s10337-012-2196-6
ER  - 
@article{
author = "Rakić, Tijana and Malenović, Anđelija and Jančić-Stojanović, Biljana and Ivanović, Darko and Medenica, Mirjana",
year = "2012",
abstract = "The algorithm of Dong and error estimation based on a priori declared negligible effects (dummy factor effects approach) were evaluated for testing robustness, in case they provide contradictory results. Robustness of LC method for separation of ropinirole and its impurity was determined. Plackett-Burman design was applied to unravel the significant/influential factors. Four selected responses (retention factor of ropinirole and impurity, selectivity and resolution) were analyzed by the standard algorithm of Dong and dummy factor effects approach. The interpretation of the results for retention factor of ropinirole and resolution was inconclusive, since the two applied approaches identified different significant factors. The potential false negative or false positive results were avoided reanalyzing the results by the modified approaches. Modification of the dummy factor effects approach included omitting the large dummy effects values, and modification of the algorithm of Dong included calculating the margin of error values for all different number of factors included, and then selecting the lowest one to be the critical effect. The applied reanalysis allowed final important factor identification and non-significant intervals for significant effects calculation.",
publisher = "Springer Heidelberg, Heidelberg",
journal = "Chromatographia",
title = "Avoiding the False Negative Results in LC Method Robustness Testing by Modifications of the Algorithm of Dong and Dummy Factor Effects Approach",
volume = "75",
number = "7-8",
pages = "397-401",
doi = "10.1007/s10337-012-2196-6"
}
Rakić, T., Malenović, A., Jančić-Stojanović, B., Ivanović, D.,& Medenica, M.. (2012). Avoiding the False Negative Results in LC Method Robustness Testing by Modifications of the Algorithm of Dong and Dummy Factor Effects Approach. in Chromatographia
Springer Heidelberg, Heidelberg., 75(7-8), 397-401.
https://doi.org/10.1007/s10337-012-2196-6
Rakić T, Malenović A, Jančić-Stojanović B, Ivanović D, Medenica M. Avoiding the False Negative Results in LC Method Robustness Testing by Modifications of the Algorithm of Dong and Dummy Factor Effects Approach. in Chromatographia. 2012;75(7-8):397-401.
doi:10.1007/s10337-012-2196-6 .
Rakić, Tijana, Malenović, Anđelija, Jančić-Stojanović, Biljana, Ivanović, Darko, Medenica, Mirjana, "Avoiding the False Negative Results in LC Method Robustness Testing by Modifications of the Algorithm of Dong and Dummy Factor Effects Approach" in Chromatographia, 75, no. 7-8 (2012):397-401,
https://doi.org/10.1007/s10337-012-2196-6 . .
5
4
5

Assessment of beta-lactams retention in hydrophilic interaction chromatography applying Box-Behnken Design

Jovanović, Marko; Rakić, Tijana; Jančić-Stojanović, Biljana; Malenović, Anđelija; Ivanović, Darko; Medenica, Mirjana

(Wiley-VCH Verlag GMBH, Weinheim, 2012)

TY  - JOUR
AU  - Jovanović, Marko
AU  - Rakić, Tijana
AU  - Jančić-Stojanović, Biljana
AU  - Malenović, Anđelija
AU  - Ivanović, Darko
AU  - Medenica, Mirjana
PY  - 2012
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/1714
AB  - In this paper, the retention prediction models for mixture of beta-lactam antibiotics analyzed by hydrophilic interaction chromatography (HILIC) are presented. The aim of the study was to investigate the retention behavior of some organic acids and amphoteric compounds including cephalosporins (cefotaxime, cefalexin, cefaclor, cefuroxime, and cefuroxime axetil) and penicillins (ampicillin and amoxicillin). Retention of substances with acidic functional group in HILIC is considered to be interesting since the majority of publications in literature are related to basic compounds. In the beginning of the study, classical silica columns were chosen for the retention analysis. Then, preliminary study was done and factors with the most significant influence on the retention factors were selected. These factors with the impact on the retention factors were investigated employing Box-Behnken design as a tool. On the basis of the obtained results the mathematical models were created and tested using ANOVA test and finally verified. This approach enables the presentation of chromatographic retention in many ways (three-dimensional (3-D) graphs and simple two-dimensional graphical presentations). All of these gave the possibility to predict the chromatographic retention under different conditions. Furthermore, regarding the structure of the analyzed compounds, the potential retention mechanisms in HILIC were suggested.
PB  - Wiley-VCH Verlag GMBH, Weinheim
T2  - Journal of Separation Science
T1  - Assessment of beta-lactams retention in hydrophilic interaction chromatography applying Box-Behnken Design
VL  - 35
IS  - 12
SP  - 1424
EP  - 1431
DO  - 10.1002/jssc.201200099
ER  - 
@article{
author = "Jovanović, Marko and Rakić, Tijana and Jančić-Stojanović, Biljana and Malenović, Anđelija and Ivanović, Darko and Medenica, Mirjana",
year = "2012",
abstract = "In this paper, the retention prediction models for mixture of beta-lactam antibiotics analyzed by hydrophilic interaction chromatography (HILIC) are presented. The aim of the study was to investigate the retention behavior of some organic acids and amphoteric compounds including cephalosporins (cefotaxime, cefalexin, cefaclor, cefuroxime, and cefuroxime axetil) and penicillins (ampicillin and amoxicillin). Retention of substances with acidic functional group in HILIC is considered to be interesting since the majority of publications in literature are related to basic compounds. In the beginning of the study, classical silica columns were chosen for the retention analysis. Then, preliminary study was done and factors with the most significant influence on the retention factors were selected. These factors with the impact on the retention factors were investigated employing Box-Behnken design as a tool. On the basis of the obtained results the mathematical models were created and tested using ANOVA test and finally verified. This approach enables the presentation of chromatographic retention in many ways (three-dimensional (3-D) graphs and simple two-dimensional graphical presentations). All of these gave the possibility to predict the chromatographic retention under different conditions. Furthermore, regarding the structure of the analyzed compounds, the potential retention mechanisms in HILIC were suggested.",
publisher = "Wiley-VCH Verlag GMBH, Weinheim",
journal = "Journal of Separation Science",
title = "Assessment of beta-lactams retention in hydrophilic interaction chromatography applying Box-Behnken Design",
volume = "35",
number = "12",
pages = "1424-1431",
doi = "10.1002/jssc.201200099"
}
Jovanović, M., Rakić, T., Jančić-Stojanović, B., Malenović, A., Ivanović, D.,& Medenica, M.. (2012). Assessment of beta-lactams retention in hydrophilic interaction chromatography applying Box-Behnken Design. in Journal of Separation Science
Wiley-VCH Verlag GMBH, Weinheim., 35(12), 1424-1431.
https://doi.org/10.1002/jssc.201200099
Jovanović M, Rakić T, Jančić-Stojanović B, Malenović A, Ivanović D, Medenica M. Assessment of beta-lactams retention in hydrophilic interaction chromatography applying Box-Behnken Design. in Journal of Separation Science. 2012;35(12):1424-1431.
doi:10.1002/jssc.201200099 .
Jovanović, Marko, Rakić, Tijana, Jančić-Stojanović, Biljana, Malenović, Anđelija, Ivanović, Darko, Medenica, Mirjana, "Assessment of beta-lactams retention in hydrophilic interaction chromatography applying Box-Behnken Design" in Journal of Separation Science, 35, no. 12 (2012):1424-1431,
https://doi.org/10.1002/jssc.201200099 . .
11
12
12

Demasking large dummy effects approach in revealing important interactions in Plackett-Burman experimental design

Rakić, Tijana; Jančić-Stojanović, Biljana; Malenović, Anđelija; Ivanović, Darko; Medenica, Mirjana

(Wiley, Hoboken, 2012)

TY  - JOUR
AU  - Rakić, Tijana
AU  - Jančić-Stojanović, Biljana
AU  - Malenović, Anđelija
AU  - Ivanović, Darko
AU  - Medenica, Mirjana
PY  - 2012
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/1646
AB  - This paper presents a newly developed demasking large dummy effects (DDE) approach for identification of significant factor interactions in Plackett-Burman experimental design. Dummy factors, as imaginary factors, are not expected to contribute to the model, so the appearance of their high effect values could indicate the significance of the interactions they are confounded with. DDE approach consists of the screening of the large estimable effects, the calculation of the interactions that contribute the most to the large dummy effects from the alias matrix, and a single pass of all subsets regressions including preselected interactions and main factors for the final model tuning. Tested on experimentally obtained data from a robustness analysis of a method for the determination of raloxifene and its four impurities, DDE approach showed to create the models that have greater statistical power than the ones described with the main factors only, which makes them more reliable and accurate for the application. Additionally, because of the interactions selection criterion and final tuning phase of the strategy, DDE approach allows the creation of models that are likely to better describe the real systems, which increases the practical value. Copyright
PB  - Wiley, Hoboken
T2  - Journal of Chemometrics
T1  - Demasking large dummy effects approach in revealing important interactions in Plackett-Burman experimental design
VL  - 26
IS  - 10
SP  - 518
EP  - 525
DO  - 10.1002/cem.2461
ER  - 
@article{
author = "Rakić, Tijana and Jančić-Stojanović, Biljana and Malenović, Anđelija and Ivanović, Darko and Medenica, Mirjana",
year = "2012",
abstract = "This paper presents a newly developed demasking large dummy effects (DDE) approach for identification of significant factor interactions in Plackett-Burman experimental design. Dummy factors, as imaginary factors, are not expected to contribute to the model, so the appearance of their high effect values could indicate the significance of the interactions they are confounded with. DDE approach consists of the screening of the large estimable effects, the calculation of the interactions that contribute the most to the large dummy effects from the alias matrix, and a single pass of all subsets regressions including preselected interactions and main factors for the final model tuning. Tested on experimentally obtained data from a robustness analysis of a method for the determination of raloxifene and its four impurities, DDE approach showed to create the models that have greater statistical power than the ones described with the main factors only, which makes them more reliable and accurate for the application. Additionally, because of the interactions selection criterion and final tuning phase of the strategy, DDE approach allows the creation of models that are likely to better describe the real systems, which increases the practical value. Copyright",
publisher = "Wiley, Hoboken",
journal = "Journal of Chemometrics",
title = "Demasking large dummy effects approach in revealing important interactions in Plackett-Burman experimental design",
volume = "26",
number = "10",
pages = "518-525",
doi = "10.1002/cem.2461"
}
Rakić, T., Jančić-Stojanović, B., Malenović, A., Ivanović, D.,& Medenica, M.. (2012). Demasking large dummy effects approach in revealing important interactions in Plackett-Burman experimental design. in Journal of Chemometrics
Wiley, Hoboken., 26(10), 518-525.
https://doi.org/10.1002/cem.2461
Rakić T, Jančić-Stojanović B, Malenović A, Ivanović D, Medenica M. Demasking large dummy effects approach in revealing important interactions in Plackett-Burman experimental design. in Journal of Chemometrics. 2012;26(10):518-525.
doi:10.1002/cem.2461 .
Rakić, Tijana, Jančić-Stojanović, Biljana, Malenović, Anđelija, Ivanović, Darko, Medenica, Mirjana, "Demasking large dummy effects approach in revealing important interactions in Plackett-Burman experimental design" in Journal of Chemometrics, 26, no. 10 (2012):518-525,
https://doi.org/10.1002/cem.2461 . .
7
4
4

Improved chromatographic response function in HILIC analysis: Application to mixture of antidepressants

Rakić, Tijana; Jančić-Stojanović, Biljana; Malenović, Anđelija; Ivanović, Darko; Medenica, Mirjana

(Elsevier Science BV, Amsterdam, 2012)

TY  - JOUR
AU  - Rakić, Tijana
AU  - Jančić-Stojanović, Biljana
AU  - Malenović, Anđelija
AU  - Ivanović, Darko
AU  - Medenica, Mirjana
PY  - 2012
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/1645
AB  - This paper presents exploration of chromatographic behavior in HILIC system by experimental design and improved chromatographic response function denoted as N-CRF*. As a model mixture six antidepressants were chosen: selegiline, mianserine, sertraline, moclobemide, fluoxetine and maprotiline. Due to complexity of retention mechanisms in HILIC system, detailed examination of experimental space assessing the influence of important factors (acetonitrile content in the mobile phase, buffer concentration and pH of the mobile phase) and their interactions was done by applying 3(3) experimental design. N-CRF*. is developed and designed to be the only output of the system which simultaneously measures the separation of all the examined substances, the chromatographic run duration and the quality of the obtained peaks shape. It allowed objective estimation of overall chromatogram quality and excluded the arbitrary judgment in ambiguous situations. The applied function highlighted the influence of investigated factors on entire mixture and enabled identification of experimental regions where the chromatographic behavior was satisfactory. Applied experimental design strategy combined with N-CRF* proved to be valuable assistance in HILIC separation of complex mixtures.
PB  - Elsevier Science BV, Amsterdam
T2  - Talanta
T1  - Improved chromatographic response function in HILIC analysis: Application to mixture of antidepressants
VL  - 98
SP  - 54
EP  - 61
DO  - 10.1016/j.talanta.2012.06.040
ER  - 
@article{
author = "Rakić, Tijana and Jančić-Stojanović, Biljana and Malenović, Anđelija and Ivanović, Darko and Medenica, Mirjana",
year = "2012",
abstract = "This paper presents exploration of chromatographic behavior in HILIC system by experimental design and improved chromatographic response function denoted as N-CRF*. As a model mixture six antidepressants were chosen: selegiline, mianserine, sertraline, moclobemide, fluoxetine and maprotiline. Due to complexity of retention mechanisms in HILIC system, detailed examination of experimental space assessing the influence of important factors (acetonitrile content in the mobile phase, buffer concentration and pH of the mobile phase) and their interactions was done by applying 3(3) experimental design. N-CRF*. is developed and designed to be the only output of the system which simultaneously measures the separation of all the examined substances, the chromatographic run duration and the quality of the obtained peaks shape. It allowed objective estimation of overall chromatogram quality and excluded the arbitrary judgment in ambiguous situations. The applied function highlighted the influence of investigated factors on entire mixture and enabled identification of experimental regions where the chromatographic behavior was satisfactory. Applied experimental design strategy combined with N-CRF* proved to be valuable assistance in HILIC separation of complex mixtures.",
publisher = "Elsevier Science BV, Amsterdam",
journal = "Talanta",
title = "Improved chromatographic response function in HILIC analysis: Application to mixture of antidepressants",
volume = "98",
pages = "54-61",
doi = "10.1016/j.talanta.2012.06.040"
}
Rakić, T., Jančić-Stojanović, B., Malenović, A., Ivanović, D.,& Medenica, M.. (2012). Improved chromatographic response function in HILIC analysis: Application to mixture of antidepressants. in Talanta
Elsevier Science BV, Amsterdam., 98, 54-61.
https://doi.org/10.1016/j.talanta.2012.06.040
Rakić T, Jančić-Stojanović B, Malenović A, Ivanović D, Medenica M. Improved chromatographic response function in HILIC analysis: Application to mixture of antidepressants. in Talanta. 2012;98:54-61.
doi:10.1016/j.talanta.2012.06.040 .
Rakić, Tijana, Jančić-Stojanović, Biljana, Malenović, Anđelija, Ivanović, Darko, Medenica, Mirjana, "Improved chromatographic response function in HILIC analysis: Application to mixture of antidepressants" in Talanta, 98 (2012):54-61,
https://doi.org/10.1016/j.talanta.2012.06.040 . .
22
18
19

Validation of an Oil-in-Water Microemulsion Liquid Chromatography Method for Analysis of Perindopril tert-Butylamine and Its Impurities

Masković, Marija; Dotsikas, Yannis; Malenović, Anđelija; Jančić-Stojanović, Biljana; Ivanović, Darko; Medenica, Mirjana

(AOAC Int, Gaithersburg, 2011)

TY  - JOUR
AU  - Masković, Marija
AU  - Dotsikas, Yannis
AU  - Malenović, Anđelija
AU  - Jančić-Stojanović, Biljana
AU  - Ivanović, Darko
AU  - Medenica, Mirjana
PY  - 2011
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/1560
AB  - This paper describes the development and validation of a microemulsion liquid chromatography (MELC) method for simultaneous determination of perindopril tert-butylamine and its impurities in bulk active substances and the pharmaceutical dosage form of tablets. An appropriate resolution with reasonable retention times was obtained for a microemulsion containing 0.24% (w/v) butyl acetate, 0.30% (w/v) ethyl acetate, 2% (w/v) sodium dodecyl sulfate, 7.75% (w/v) n-butanol, and 20.0 mM potassium dihydrogen phosphate, the pH of which was adjusted to 3.70 with 85% orthophosphoric acid. Separations were performed on a Nucleosil 120-5 butyl modified (C4), 250 x 4 mm, 5 pm particle size silica column at 40 degrees C, with a mobile phase flow rate of 1.25 mL/min. UV detection was performed at 254 nm. The established method was subjected to method validation, and required validation parameters were defined. Robustness testing, an important part of method validation, was performed as well. Since robustness validation can be conducted using different experimental designs, the Plackett-Burman design was applied due to its possibility of testing many factors at the same time. The validated MELC method was found to be suitable for the simultaneous determination of perindopril tert-butylamine and its impurities in pharmaceuticals.
PB  - AOAC Int, Gaithersburg
T2  - Journal of AOAC International
T1  - Validation of an Oil-in-Water Microemulsion Liquid Chromatography Method for Analysis of Perindopril tert-Butylamine and Its Impurities
VL  - 94
IS  - 3
SP  - 723
EP  - 734
UR  - https://hdl.handle.net/21.15107/rcub_farfar_1560
ER  - 
@article{
author = "Masković, Marija and Dotsikas, Yannis and Malenović, Anđelija and Jančić-Stojanović, Biljana and Ivanović, Darko and Medenica, Mirjana",
year = "2011",
abstract = "This paper describes the development and validation of a microemulsion liquid chromatography (MELC) method for simultaneous determination of perindopril tert-butylamine and its impurities in bulk active substances and the pharmaceutical dosage form of tablets. An appropriate resolution with reasonable retention times was obtained for a microemulsion containing 0.24% (w/v) butyl acetate, 0.30% (w/v) ethyl acetate, 2% (w/v) sodium dodecyl sulfate, 7.75% (w/v) n-butanol, and 20.0 mM potassium dihydrogen phosphate, the pH of which was adjusted to 3.70 with 85% orthophosphoric acid. Separations were performed on a Nucleosil 120-5 butyl modified (C4), 250 x 4 mm, 5 pm particle size silica column at 40 degrees C, with a mobile phase flow rate of 1.25 mL/min. UV detection was performed at 254 nm. The established method was subjected to method validation, and required validation parameters were defined. Robustness testing, an important part of method validation, was performed as well. Since robustness validation can be conducted using different experimental designs, the Plackett-Burman design was applied due to its possibility of testing many factors at the same time. The validated MELC method was found to be suitable for the simultaneous determination of perindopril tert-butylamine and its impurities in pharmaceuticals.",
publisher = "AOAC Int, Gaithersburg",
journal = "Journal of AOAC International",
title = "Validation of an Oil-in-Water Microemulsion Liquid Chromatography Method for Analysis of Perindopril tert-Butylamine and Its Impurities",
volume = "94",
number = "3",
pages = "723-734",
url = "https://hdl.handle.net/21.15107/rcub_farfar_1560"
}
Masković, M., Dotsikas, Y., Malenović, A., Jančić-Stojanović, B., Ivanović, D.,& Medenica, M.. (2011). Validation of an Oil-in-Water Microemulsion Liquid Chromatography Method for Analysis of Perindopril tert-Butylamine and Its Impurities. in Journal of AOAC International
AOAC Int, Gaithersburg., 94(3), 723-734.
https://hdl.handle.net/21.15107/rcub_farfar_1560
Masković M, Dotsikas Y, Malenović A, Jančić-Stojanović B, Ivanović D, Medenica M. Validation of an Oil-in-Water Microemulsion Liquid Chromatography Method for Analysis of Perindopril tert-Butylamine and Its Impurities. in Journal of AOAC International. 2011;94(3):723-734.
https://hdl.handle.net/21.15107/rcub_farfar_1560 .
Masković, Marija, Dotsikas, Yannis, Malenović, Anđelija, Jančić-Stojanović, Biljana, Ivanović, Darko, Medenica, Mirjana, "Validation of an Oil-in-Water Microemulsion Liquid Chromatography Method for Analysis of Perindopril tert-Butylamine and Its Impurities" in Journal of AOAC International, 94, no. 3 (2011):723-734,
https://hdl.handle.net/21.15107/rcub_farfar_1560 .
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10