Multicriteria optimization methodology in development of HPLC separation of mycophenolic acid and mycophenolic acid glucuronide in human urine and plasma
Само за регистроване кориснике
2009
Чланак у часопису (Објављена верзија)
Метаподаци
Приказ свих података о документуАпстракт
Multicriteria optimization methodology was applied for development of isocratic reversed-phased HPLC method for simultaneous determination of mycophenolic acid (MPA) and mycophenolic acid glucuronide (MPAG) in human urine and plasma. In the first stage of method development, pH value of the water phase. percentage of acetonitrile, temperature of the column and flow rate of the mobile phase were investigated using fractional factorial design. Afterwards, the optimal conditions were found employing central composite design and Derringer's desirability function. Two goals were considered, the retention factor of the MPAG to be in the range, between 0.8 and 1.118 which allowed well separation of MPAG from the urine and plasma peaks, and the shortest possible total analysis run time. Then, the obtained sigmoid functions were used to transform the optimization criteria into the desirability values. The satisfactory chromatographic conditions were obtained with mobile phase consisted of aceto...nitrile-phosphate buffer (pH 2.4; 0.04 M KH2PO4) (28:72, v/v). The separation was performed on C-18 Chromolith column (100 mm x 4.6 mm) with flow rate of 5 mL/min, the temperature of the column was 25 degrees C and the chosen wavelength for simultaneous determination of MPA and MPAG was 215 nm. The MPAG eluted at 0.552 min and the duration of run was 3.092 min. Afterwards, the method was subjected to validation. Linearity was observed over the concentration range of 1-50 mu g/mL for MPA and 1-500 mu g/mL for MPAG in urine and 1-60 mu g/mL for MPA and 1-70 mu g/mL for MPAG in plasma matrix. The method showed intra-day and inter-day precision with relative standard deviation lower then 5% and accuracy as recovery (%) between 100 +/- 5%.
Кључне речи:
Mycophenolic acid / Mycophenolic acid glucuronide / Experimental design / Derringer's desirability functionИзвор:
Journal of Pharmaceutical and Biomedical Analysis, 2009, 50, 4, 640-648Издавач:
- Elsevier Science BV, Amsterdam
Финансирање / пројекти:
- Синтеза, квантитативни односи између структуре/особина и активности, физичко-хемијска карактеризација и анализа фармаколошки активних супстанци (RS-MESTD-MPN2006-2010-142071)
DOI: 10.1016/j.jpba.2008.09.052
ISSN: 0731-7085
PubMed: 19036547
WoS: 000269168300015
Scopus: 2-s2.0-67949095585
Институција/група
PharmacyTY - JOUR AU - Živanović, Ljiljana AU - Protić, Ana AU - Zečević, Mira AU - Jocić, Biljana AU - Kostić, Mirjana PY - 2009 UR - https://farfar.pharmacy.bg.ac.rs/handle/123456789/1255 AB - Multicriteria optimization methodology was applied for development of isocratic reversed-phased HPLC method for simultaneous determination of mycophenolic acid (MPA) and mycophenolic acid glucuronide (MPAG) in human urine and plasma. In the first stage of method development, pH value of the water phase. percentage of acetonitrile, temperature of the column and flow rate of the mobile phase were investigated using fractional factorial design. Afterwards, the optimal conditions were found employing central composite design and Derringer's desirability function. Two goals were considered, the retention factor of the MPAG to be in the range, between 0.8 and 1.118 which allowed well separation of MPAG from the urine and plasma peaks, and the shortest possible total analysis run time. Then, the obtained sigmoid functions were used to transform the optimization criteria into the desirability values. The satisfactory chromatographic conditions were obtained with mobile phase consisted of acetonitrile-phosphate buffer (pH 2.4; 0.04 M KH2PO4) (28:72, v/v). The separation was performed on C-18 Chromolith column (100 mm x 4.6 mm) with flow rate of 5 mL/min, the temperature of the column was 25 degrees C and the chosen wavelength for simultaneous determination of MPA and MPAG was 215 nm. The MPAG eluted at 0.552 min and the duration of run was 3.092 min. Afterwards, the method was subjected to validation. Linearity was observed over the concentration range of 1-50 mu g/mL for MPA and 1-500 mu g/mL for MPAG in urine and 1-60 mu g/mL for MPA and 1-70 mu g/mL for MPAG in plasma matrix. The method showed intra-day and inter-day precision with relative standard deviation lower then 5% and accuracy as recovery (%) between 100 +/- 5%. PB - Elsevier Science BV, Amsterdam T2 - Journal of Pharmaceutical and Biomedical Analysis T1 - Multicriteria optimization methodology in development of HPLC separation of mycophenolic acid and mycophenolic acid glucuronide in human urine and plasma VL - 50 IS - 4 SP - 640 EP - 648 DO - 10.1016/j.jpba.2008.09.052 ER -
@article{ author = "Živanović, Ljiljana and Protić, Ana and Zečević, Mira and Jocić, Biljana and Kostić, Mirjana", year = "2009", abstract = "Multicriteria optimization methodology was applied for development of isocratic reversed-phased HPLC method for simultaneous determination of mycophenolic acid (MPA) and mycophenolic acid glucuronide (MPAG) in human urine and plasma. In the first stage of method development, pH value of the water phase. percentage of acetonitrile, temperature of the column and flow rate of the mobile phase were investigated using fractional factorial design. Afterwards, the optimal conditions were found employing central composite design and Derringer's desirability function. Two goals were considered, the retention factor of the MPAG to be in the range, between 0.8 and 1.118 which allowed well separation of MPAG from the urine and plasma peaks, and the shortest possible total analysis run time. Then, the obtained sigmoid functions were used to transform the optimization criteria into the desirability values. The satisfactory chromatographic conditions were obtained with mobile phase consisted of acetonitrile-phosphate buffer (pH 2.4; 0.04 M KH2PO4) (28:72, v/v). The separation was performed on C-18 Chromolith column (100 mm x 4.6 mm) with flow rate of 5 mL/min, the temperature of the column was 25 degrees C and the chosen wavelength for simultaneous determination of MPA and MPAG was 215 nm. The MPAG eluted at 0.552 min and the duration of run was 3.092 min. Afterwards, the method was subjected to validation. Linearity was observed over the concentration range of 1-50 mu g/mL for MPA and 1-500 mu g/mL for MPAG in urine and 1-60 mu g/mL for MPA and 1-70 mu g/mL for MPAG in plasma matrix. The method showed intra-day and inter-day precision with relative standard deviation lower then 5% and accuracy as recovery (%) between 100 +/- 5%.", publisher = "Elsevier Science BV, Amsterdam", journal = "Journal of Pharmaceutical and Biomedical Analysis", title = "Multicriteria optimization methodology in development of HPLC separation of mycophenolic acid and mycophenolic acid glucuronide in human urine and plasma", volume = "50", number = "4", pages = "640-648", doi = "10.1016/j.jpba.2008.09.052" }
Živanović, L., Protić, A., Zečević, M., Jocić, B.,& Kostić, M.. (2009). Multicriteria optimization methodology in development of HPLC separation of mycophenolic acid and mycophenolic acid glucuronide in human urine and plasma. in Journal of Pharmaceutical and Biomedical Analysis Elsevier Science BV, Amsterdam., 50(4), 640-648. https://doi.org/10.1016/j.jpba.2008.09.052
Živanović L, Protić A, Zečević M, Jocić B, Kostić M. Multicriteria optimization methodology in development of HPLC separation of mycophenolic acid and mycophenolic acid glucuronide in human urine and plasma. in Journal of Pharmaceutical and Biomedical Analysis. 2009;50(4):640-648. doi:10.1016/j.jpba.2008.09.052 .
Živanović, Ljiljana, Protić, Ana, Zečević, Mira, Jocić, Biljana, Kostić, Mirjana, "Multicriteria optimization methodology in development of HPLC separation of mycophenolic acid and mycophenolic acid glucuronide in human urine and plasma" in Journal of Pharmaceutical and Biomedical Analysis, 50, no. 4 (2009):640-648, https://doi.org/10.1016/j.jpba.2008.09.052 . .