TY  - JOUR
AU  - Otašević, Biljana
AU  - Milovanović, Svetlana
AU  - Zečević, Mira
AU  - Golubović, Jelena
AU  - Protić, Ana
PY  - 2014
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2186
AB  - A simple, rapid, isocratic, stability-indicating reverse phase ultra-performance liquid chromatographic (RP-UPLC) method was developed and validated for the routine analysis of moxonidine in the presence of its degradation products in active pharmaceutical ingredient and pharmaceutical dosage forms. Forced degradation studies were performed according to the guidance of International Conference for Harmonization and were used to evaluate moxonidine intrinsic stability. The drug was subjected to acid, neutral and base hydrolysis as well as to oxidative, thermal and photolytic decomposition in both solution and solid state. The drug appeared to be unstable towards acid and base hydrolysis. To achieve desirable conditions for UPLC analysis, the method development was done with the assistance of experimental design and multivariate optimization methodology by means of Derringer's desirability function. Stress samples were analyzed according to the experimental plan for fractional factorial screening design and Box-Behnken optimization design. The chromatographic separation was achieved on a C-18 Hypersil Gold aq. column (100 mm x 2.1 mm, 1.9 mu m) with the mobile phase consisting of methanol-ammonium acetate buffer (10 mM, pH 3.43) mixture (0.9:99.1, v/v) pumped at a flow rate of 870 mu L min(-1) and detection wavelength of 255 nm. The UPLC-MS and UPLC-MS/MS analyses were further used to characterize the found degradation products. The validation of the proposed method was also performed considering selectivity, linearity, accuracy, precision, limit of detection and limit of quantification, and the results indicated that the method fulfilled all required criteria. The method was successfully applied to the analysis of commercial tablets.
PB  - Springer Heidelberg, Heidelberg
T2  - Chromatographia
T1  - UPLC Method for Determination of Moxonidine and Its Degradation Products in Active Pharmaceutical Ingredient and Pharmaceutical Dosage Form
VL  - 77
IS  - 1-2
SP  - 109
EP  - 118
DO  - 10.1007/s10337-013-2580-x
ER  - 

@article{
author = "Otašević, Biljana and Milovanović, Svetlana and Zečević, Mira and Golubović, Jelena and Protić, Ana",
year = "2014",
abstract = "A simple, rapid, isocratic, stability-indicating reverse phase ultra-performance liquid chromatographic (RP-UPLC) method was developed and validated for the routine analysis of moxonidine in the presence of its degradation products in active pharmaceutical ingredient and pharmaceutical dosage forms. Forced degradation studies were performed according to the guidance of International Conference for Harmonization and were used to evaluate moxonidine intrinsic stability. The drug was subjected to acid, neutral and base hydrolysis as well as to oxidative, thermal and photolytic decomposition in both solution and solid state. The drug appeared to be unstable towards acid and base hydrolysis. To achieve desirable conditions for UPLC analysis, the method development was done with the assistance of experimental design and multivariate optimization methodology by means of Derringer's desirability function. Stress samples were analyzed according to the experimental plan for fractional factorial screening design and Box-Behnken optimization design. The chromatographic separation was achieved on a C-18 Hypersil Gold aq. column (100 mm x 2.1 mm, 1.9 mu m) with the mobile phase consisting of methanol-ammonium acetate buffer (10 mM, pH 3.43) mixture (0.9:99.1, v/v) pumped at a flow rate of 870 mu L min(-1) and detection wavelength of 255 nm. The UPLC-MS and UPLC-MS/MS analyses were further used to characterize the found degradation products. The validation of the proposed method was also performed considering selectivity, linearity, accuracy, precision, limit of detection and limit of quantification, and the results indicated that the method fulfilled all required criteria. The method was successfully applied to the analysis of commercial tablets.",
publisher = "Springer Heidelberg, Heidelberg",
journal = "Chromatographia",
title = "UPLC Method for Determination of Moxonidine and Its Degradation Products in Active Pharmaceutical Ingredient and Pharmaceutical Dosage Form",
volume = "77",
number = "1-2",
pages = "109-118",
doi = "10.1007/s10337-013-2580-x"
}

Otašević, B., Milovanović, S., Zečević, M., Golubović, J.,& Protić, A.. (2014). UPLC Method for Determination of Moxonidine and Its Degradation Products in Active Pharmaceutical Ingredient and Pharmaceutical Dosage Form. in Chromatographia
Springer Heidelberg, Heidelberg., 77(1-2), 109-118.
https://doi.org/10.1007/s10337-013-2580-x

Otašević B, Milovanović S, Zečević M, Golubović J, Protić A. UPLC Method for Determination of Moxonidine and Its Degradation Products in Active Pharmaceutical Ingredient and Pharmaceutical Dosage Form. in Chromatographia. 2014;77(1-2):109-118.
doi:10.1007/s10337-013-2580-x .

Otašević, Biljana, Milovanović, Svetlana, Zečević, Mira, Golubović, Jelena, Protić, Ana, "UPLC Method for Determination of Moxonidine and Its Degradation Products in Active Pharmaceutical Ingredient and Pharmaceutical Dosage Form" in Chromatographia, 77, no. 1-2 (2014):109-118,
https://doi.org/10.1007/s10337-013-2580-x . .

TY  - JOUR
AU  - Milovanović, Svetlana
AU  - Otašević, Biljana
AU  - Zečević, Mira
AU  - Živanović, Ljiljana
AU  - Protić, Ana
PY  - 2012
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/1710
AB  - A simple, rapid, isocratic reversed-phase high-performance liquid chromatographic method was developed and validated for the analysis of moxonidine and its impurities in tablet formulations. The chromatographic separation was achieved on a Symmetry shield C18 column (250 mm x 4.6 mm, 5 mu m) by employing a mobile phase consisting of methanol-potassium phosphate buffer (0.05 M) mixture (15:85, v/v) (pH 3.5) at a flow rate of 1 ml min(-1): detection at 255 nm. Central composite design technique and response surface method were used to evaluate the effects of variations of selected factors (buffer pH value, column temperature, methanol content) in order to achieve the best isocratic separation within short analysis time (less than 10 min), as well as for robustness test considerations. The method fulfilled the validation criteria: specificity, linearity, accuracy, precision, limit of detection and limit of quantitation. The method was successfully applied for the analysis of commercial moxonidine tablets.
PB  - Elsevier Science BV, Amsterdam
T2  - Journal of Pharmaceutical and Biomedical Analysis
T1  - Development and validation of reversed phase high performance liquid chromatographic method for determination of moxonidine in the presence of its impurities
VL  - 59
SP  - 151
EP  - 156
DO  - 10.1016/j.jpba.2011.09.029
ER  - 

@article{
author = "Milovanović, Svetlana and Otašević, Biljana and Zečević, Mira and Živanović, Ljiljana and Protić, Ana",
year = "2012",
abstract = "A simple, rapid, isocratic reversed-phase high-performance liquid chromatographic method was developed and validated for the analysis of moxonidine and its impurities in tablet formulations. The chromatographic separation was achieved on a Symmetry shield C18 column (250 mm x 4.6 mm, 5 mu m) by employing a mobile phase consisting of methanol-potassium phosphate buffer (0.05 M) mixture (15:85, v/v) (pH 3.5) at a flow rate of 1 ml min(-1): detection at 255 nm. Central composite design technique and response surface method were used to evaluate the effects of variations of selected factors (buffer pH value, column temperature, methanol content) in order to achieve the best isocratic separation within short analysis time (less than 10 min), as well as for robustness test considerations. The method fulfilled the validation criteria: specificity, linearity, accuracy, precision, limit of detection and limit of quantitation. The method was successfully applied for the analysis of commercial moxonidine tablets.",
publisher = "Elsevier Science BV, Amsterdam",
journal = "Journal of Pharmaceutical and Biomedical Analysis",
title = "Development and validation of reversed phase high performance liquid chromatographic method for determination of moxonidine in the presence of its impurities",
volume = "59",
pages = "151-156",
doi = "10.1016/j.jpba.2011.09.029"
}

Milovanović, S., Otašević, B., Zečević, M., Živanović, L.,& Protić, A.. (2012). Development and validation of reversed phase high performance liquid chromatographic method for determination of moxonidine in the presence of its impurities. in Journal of Pharmaceutical and Biomedical Analysis
Elsevier Science BV, Amsterdam., 59, 151-156.
https://doi.org/10.1016/j.jpba.2011.09.029

Milovanović S, Otašević B, Zečević M, Živanović L, Protić A. Development and validation of reversed phase high performance liquid chromatographic method for determination of moxonidine in the presence of its impurities. in Journal of Pharmaceutical and Biomedical Analysis. 2012;59:151-156.
doi:10.1016/j.jpba.2011.09.029 .

Milovanović, Svetlana, Otašević, Biljana, Zečević, Mira, Živanović, Ljiljana, Protić, Ana, "Development and validation of reversed phase high performance liquid chromatographic method for determination of moxonidine in the presence of its impurities" in Journal of Pharmaceutical and Biomedical Analysis, 59 (2012):151-156,
https://doi.org/10.1016/j.jpba.2011.09.029 . .