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 .

TY  - JOUR
AU  - Malenović, Anđelija
AU  - Dotsikas, Yannis
AU  - Masković, Marija
AU  - Jančić-Stojanović, Biljana
AU  - Ivanović, Darko
AU  - Medenica, Mirjana
PY  - 2011
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/1456
AB  - In the current paper the application of multiobjective optimization (MOOP) technique, via Derringer's desirability function, to a microemulsion liquid chromatographic (MELC) method is described. Chromatographic separation of perindopril tert-butylamine and its four impurities was selected as the case study. Central composite design (CCD) with fractional factorial design, +/- 0.5 alpha star design and four replications in central point was applied for a response surface study, in order to examine in depth the effects of the most important factors. As factors that influence the system mostly (i) content of ethyl acetate and (ii) butyl acetate in composite internal phase, (iii) content of sodium dodecyl sulfate (surfactant) and (iv) n-butanol (co-surfactant). as well as (v) pH of the mobile phase were selected. Retention factor of (a) perindoprilat and (b) impurity Y 31 and
PB  - Elsevier Science BV, Amsterdam
T2  - Microchemical Journal
T1  - Desirability-based optimization and its sensitivity analysis for the perindopril and its impurities analysis in a microemulsion LC system
VL  - 99
IS  - 2
SP  - 454
EP  - 460
DO  - 10.1016/j.microc.2011.06.022
ER  - 

@article{
author = "Malenović, Anđelija and Dotsikas, Yannis and Masković, Marija and Jančić-Stojanović, Biljana and Ivanović, Darko and Medenica, Mirjana",
year = "2011",
abstract = "In the current paper the application of multiobjective optimization (MOOP) technique, via Derringer's desirability function, to a microemulsion liquid chromatographic (MELC) method is described. Chromatographic separation of perindopril tert-butylamine and its four impurities was selected as the case study. Central composite design (CCD) with fractional factorial design, +/- 0.5 alpha star design and four replications in central point was applied for a response surface study, in order to examine in depth the effects of the most important factors. As factors that influence the system mostly (i) content of ethyl acetate and (ii) butyl acetate in composite internal phase, (iii) content of sodium dodecyl sulfate (surfactant) and (iv) n-butanol (co-surfactant). as well as (v) pH of the mobile phase were selected. Retention factor of (a) perindoprilat and (b) impurity Y 31 and",
publisher = "Elsevier Science BV, Amsterdam",
journal = "Microchemical Journal",
title = "Desirability-based optimization and its sensitivity analysis for the perindopril and its impurities analysis in a microemulsion LC system",
volume = "99",
number = "2",
pages = "454-460",
doi = "10.1016/j.microc.2011.06.022"
}

Malenović, A., Dotsikas, Y., Masković, M., Jančić-Stojanović, B., Ivanović, D.,& Medenica, M.. (2011). Desirability-based optimization and its sensitivity analysis for the perindopril and its impurities analysis in a microemulsion LC system. in Microchemical Journal
Elsevier Science BV, Amsterdam., 99(2), 454-460.
https://doi.org/10.1016/j.microc.2011.06.022

Malenović A, Dotsikas Y, Masković M, Jančić-Stojanović B, Ivanović D, Medenica M. Desirability-based optimization and its sensitivity analysis for the perindopril and its impurities analysis in a microemulsion LC system. in Microchemical Journal. 2011;99(2):454-460.
doi:10.1016/j.microc.2011.06.022 .

Malenović, Anđelija, Dotsikas, Yannis, Masković, Marija, Jančić-Stojanović, Biljana, Ivanović, Darko, Medenica, Mirjana, "Desirability-based optimization and its sensitivity analysis for the perindopril and its impurities analysis in a microemulsion LC system" in Microchemical Journal, 99, no. 2 (2011):454-460,
https://doi.org/10.1016/j.microc.2011.06.022 . .

TY  - JOUR
AU  - Ivanović, Darko
AU  - Malenović, Anđelija
AU  - Jančić, Biljana
AU  - Medenica, Mirjana
AU  - Masković, Marija
PY  - 2007
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/941
AB  - The multi-component preparation Co -Diovan (R) is indicated for the hypertension treatment in patients whose blood pressure is not adequately controlled by monotherapy. Its active ingredients are valsartan and hydrochlorothiazide. The reversed-phase high performance liquid chromatographic method (RP -HPLC) for the determination of valsartan and hydrochlorothiazide, as well as their impurities level, was developed and described in this paper. As the investigated substances were structurally different with extremely different lipophilicity and polarity, isocratic elution was not possible, so an optimal gradient mode was settled on. The chromatograms were recorded using the Agilent 1100 Series chromatographic system with DAD detector. Separations were performed on a Hypersil 120-5 ODS column (250 mm x 4.6 mm; 5 mm particle size) at 25 degrees C column temperature. The gradient high performance liquid chromatographic system was developed, and the following mobile phases were used: A) mixture acetonitrile -water (10: 90 V/V); pH of the mobile phase was adjusted to 2.5 with 85% orthophosphoric acid, and B) mixture acetonitrile -water (90: 10 V/V); pH of the mobile phase was adjusted to 2.5 with 85% orthophosphoric acid. Injection volume was 50 mu L, flow rate 1 mL min(-1) and UV detection was performed at 256 nm. Methyl parahydroxybenzoate was used as an internal standard and acetonitrile-water (40:60 V/V) as a solvent. Afterwards, the developed method was subjected to the method validation. The investigated validation parameters (selectivity, linearity, precision, accuracy, LOQ, and LOD) proved the suitability of the method for the simultaneous determination of valsartan, hydrochlorothiazide, and their impurities in appropriate tablets.
PB  - Taylor & Francis Inc, Philadelphia
T2  - Journal of Liquid Chromatography & Related Technologies
T1  - Monitoring of impurity level of valsartan and hydrochlorothiazide employing an RP-HPLC gradient mode
VL  - 30
IS  - 19
SP  - 2879
EP  - 2890
DO  - 10.1080/10826070701588638
ER  - 

@article{
author = "Ivanović, Darko and Malenović, Anđelija and Jančić, Biljana and Medenica, Mirjana and Masković, Marija",
year = "2007",
abstract = "The multi-component preparation Co -Diovan (R) is indicated for the hypertension treatment in patients whose blood pressure is not adequately controlled by monotherapy. Its active ingredients are valsartan and hydrochlorothiazide. The reversed-phase high performance liquid chromatographic method (RP -HPLC) for the determination of valsartan and hydrochlorothiazide, as well as their impurities level, was developed and described in this paper. As the investigated substances were structurally different with extremely different lipophilicity and polarity, isocratic elution was not possible, so an optimal gradient mode was settled on. The chromatograms were recorded using the Agilent 1100 Series chromatographic system with DAD detector. Separations were performed on a Hypersil 120-5 ODS column (250 mm x 4.6 mm; 5 mm particle size) at 25 degrees C column temperature. The gradient high performance liquid chromatographic system was developed, and the following mobile phases were used: A) mixture acetonitrile -water (10: 90 V/V); pH of the mobile phase was adjusted to 2.5 with 85% orthophosphoric acid, and B) mixture acetonitrile -water (90: 10 V/V); pH of the mobile phase was adjusted to 2.5 with 85% orthophosphoric acid. Injection volume was 50 mu L, flow rate 1 mL min(-1) and UV detection was performed at 256 nm. Methyl parahydroxybenzoate was used as an internal standard and acetonitrile-water (40:60 V/V) as a solvent. Afterwards, the developed method was subjected to the method validation. The investigated validation parameters (selectivity, linearity, precision, accuracy, LOQ, and LOD) proved the suitability of the method for the simultaneous determination of valsartan, hydrochlorothiazide, and their impurities in appropriate tablets.",
publisher = "Taylor & Francis Inc, Philadelphia",
journal = "Journal of Liquid Chromatography & Related Technologies",
title = "Monitoring of impurity level of valsartan and hydrochlorothiazide employing an RP-HPLC gradient mode",
volume = "30",
number = "19",
pages = "2879-2890",
doi = "10.1080/10826070701588638"
}

Ivanović, D., Malenović, A., Jančić, B., Medenica, M.,& Masković, M.. (2007). Monitoring of impurity level of valsartan and hydrochlorothiazide employing an RP-HPLC gradient mode. in Journal of Liquid Chromatography & Related Technologies
Taylor & Francis Inc, Philadelphia., 30(19), 2879-2890.
https://doi.org/10.1080/10826070701588638

Ivanović D, Malenović A, Jančić B, Medenica M, Masković M. Monitoring of impurity level of valsartan and hydrochlorothiazide employing an RP-HPLC gradient mode. in Journal of Liquid Chromatography & Related Technologies. 2007;30(19):2879-2890.
doi:10.1080/10826070701588638 .

Ivanović, Darko, Malenović, Anđelija, Jančić, Biljana, Medenica, Mirjana, Masković, Marija, "Monitoring of impurity level of valsartan and hydrochlorothiazide employing an RP-HPLC gradient mode" in Journal of Liquid Chromatography & Related Technologies, 30, no. 19 (2007):2879-2890,
https://doi.org/10.1080/10826070701588638 . .