A Validated Enantiospecific Method for Determination and Purity Assay of Clopridogrel
Abstract
A new and accurate HPLC method using beta-cyclodextrin chemically bonded to spherical silica particles as chiral stationary phase (CSP) was developed and validated for determination of S-clopidogrel and its impurities R-enantiomer and S-acid as a hydrolytic product. The effects of acetonitrile and methanol content in the mobile phase and temperature on the resolution and retention of enantiomers were investigated. A satisfactory resolution of S-clopidogrel active form and its impurities was achieved on ChiraDex(R) column (5 mu m, 4 x 250 mm) at a flow rate of 1.0 ml/min and 17 degrees C using acetonitrile, methanol and 0.01 M potassium dihydrogen phosphate solution (15:5:80 v/v/v) as mobile phase. The detection wavelength was set at 220 nm. The method was validated in terms of accuracy, precision, linearity, and robustness. The limit of detection for R-enantiomer and S-acid were 0.75 and 0.09 mu g/ml, respectively, injection volume being 20 mu l. Finally, the molecular modeling of the ...inclusion complexes between the analytes and beta-cyclodextrin was performed to investigate the mechanism of the enantiorecognition and to study the quantitative structure-retention relationships. Chirality 21:878-885, 2009.
Keywords:
clopidogrel / chiral separation / cyclodextrin-based chiral stationary phase / enantiomeric impuritySource:
Chirality, 2009, 21, 10, 878-885Publisher:
- Wiley, Hoboken
Funding / projects:
- Sinteza, kvantitativni odnosi između strukture/osobina i aktivnosti, fizičko-hemijska karakterizacija i analiza farmakološki aktivnih supstanci (RS-MESTD-MPN2006-2010-142071)
DOI: 10.1002/chir.20681
ISSN: 0899-0042
PubMed: 19023872
WoS: 000271401800002
Scopus: 2-s2.0-70350561081
Collections
Institution/Community
PharmacyTY - JOUR AU - Nikolić, Katarina AU - Ivković, Branka AU - Besović, Željka AU - Marković, Slavko AU - Agbaba, Danica PY - 2009 UR - https://farfar.pharmacy.bg.ac.rs/handle/123456789/1202 AB - A new and accurate HPLC method using beta-cyclodextrin chemically bonded to spherical silica particles as chiral stationary phase (CSP) was developed and validated for determination of S-clopidogrel and its impurities R-enantiomer and S-acid as a hydrolytic product. The effects of acetonitrile and methanol content in the mobile phase and temperature on the resolution and retention of enantiomers were investigated. A satisfactory resolution of S-clopidogrel active form and its impurities was achieved on ChiraDex(R) column (5 mu m, 4 x 250 mm) at a flow rate of 1.0 ml/min and 17 degrees C using acetonitrile, methanol and 0.01 M potassium dihydrogen phosphate solution (15:5:80 v/v/v) as mobile phase. The detection wavelength was set at 220 nm. The method was validated in terms of accuracy, precision, linearity, and robustness. The limit of detection for R-enantiomer and S-acid were 0.75 and 0.09 mu g/ml, respectively, injection volume being 20 mu l. Finally, the molecular modeling of the inclusion complexes between the analytes and beta-cyclodextrin was performed to investigate the mechanism of the enantiorecognition and to study the quantitative structure-retention relationships. Chirality 21:878-885, 2009. PB - Wiley, Hoboken T2 - Chirality T1 - A Validated Enantiospecific Method for Determination and Purity Assay of Clopridogrel VL - 21 IS - 10 SP - 878 EP - 885 DO - 10.1002/chir.20681 ER -
@article{ author = "Nikolić, Katarina and Ivković, Branka and Besović, Željka and Marković, Slavko and Agbaba, Danica", year = "2009", abstract = "A new and accurate HPLC method using beta-cyclodextrin chemically bonded to spherical silica particles as chiral stationary phase (CSP) was developed and validated for determination of S-clopidogrel and its impurities R-enantiomer and S-acid as a hydrolytic product. The effects of acetonitrile and methanol content in the mobile phase and temperature on the resolution and retention of enantiomers were investigated. A satisfactory resolution of S-clopidogrel active form and its impurities was achieved on ChiraDex(R) column (5 mu m, 4 x 250 mm) at a flow rate of 1.0 ml/min and 17 degrees C using acetonitrile, methanol and 0.01 M potassium dihydrogen phosphate solution (15:5:80 v/v/v) as mobile phase. The detection wavelength was set at 220 nm. The method was validated in terms of accuracy, precision, linearity, and robustness. The limit of detection for R-enantiomer and S-acid were 0.75 and 0.09 mu g/ml, respectively, injection volume being 20 mu l. Finally, the molecular modeling of the inclusion complexes between the analytes and beta-cyclodextrin was performed to investigate the mechanism of the enantiorecognition and to study the quantitative structure-retention relationships. Chirality 21:878-885, 2009.", publisher = "Wiley, Hoboken", journal = "Chirality", title = "A Validated Enantiospecific Method for Determination and Purity Assay of Clopridogrel", volume = "21", number = "10", pages = "878-885", doi = "10.1002/chir.20681" }
Nikolić, K., Ivković, B., Besović, Ž., Marković, S.,& Agbaba, D.. (2009). A Validated Enantiospecific Method for Determination and Purity Assay of Clopridogrel. in Chirality Wiley, Hoboken., 21(10), 878-885. https://doi.org/10.1002/chir.20681
Nikolić K, Ivković B, Besović Ž, Marković S, Agbaba D. A Validated Enantiospecific Method for Determination and Purity Assay of Clopridogrel. in Chirality. 2009;21(10):878-885. doi:10.1002/chir.20681 .
Nikolić, Katarina, Ivković, Branka, Besović, Željka, Marković, Slavko, Agbaba, Danica, "A Validated Enantiospecific Method for Determination and Purity Assay of Clopridogrel" in Chirality, 21, no. 10 (2009):878-885, https://doi.org/10.1002/chir.20681 . .