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Journal of ZheJiang University(Medical Science)  2011, Vol. 40 Issue (1): 12-16    DOI: 10.3785/j.issn.1008-9292.2011.01.003
    
Chiral separation of fluvastatin enantiomers with in vitro cellular method
QU Bo-xuan,TIAN Ye,YU Lu-shan,JIANG Hui-di,ZHOU Quan,ZEGN Su
Department of Pharmaceutical Analysis and Drug Metabolism,College of Pharmaceutical Sciences,Zhejiang University,Hangzhou 310058,China
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Abstract  Objective: To establish a chiral separation method for determination of fluvastatin enantiomer with in vitro cellular model.
Methods: The determination was performed on Chiralpak AD column(4.6 mm×250 mm); and the phase consisted of hexane-isopropanol -trifluoroacetic acid (90∶10∶0.1) at a flow rate of 0.5 ml/min with UV detection of 239 nm.
Results: The standard curve was linear over the concentration range of 20 μmol/L-300 μmol/L (r2=0.9993,r2=0.9997). The recovery for this assay was (99.4±0.8 )%,precision for inter-assay and intra-assay was < 10%.
Conclusion: The normal-phase HPLC chiral separation method was accurate and suitable for study on the stereoselectivity of fluvastatin with in vitro cellular model.


Key wordsFluvastatin/isol      Chromatography, high pressure liquid/methods      Stereoisomerism     
Published: 25 January 2011
Cite this article:

. Chiral separation of fluvastatin enantiomers with in vitro cellular method. Journal of ZheJiang University(Medical Science), 2011, 40(1): 12-16.

URL:

https://www.zjujournals.com/med/10.3785/j.issn.1008-9292.2011.01.003     OR     https://www.zjujournals.com/med/Y2011/V40/I1/12


体外细胞模型中氟伐他汀对映体的手性分离和含量测定方法学研究

目的:建立手性固定相(CSP)正相高效液相色谱法分离细胞裂解液中氟伐他汀对映体的分析方法。
方法:采用直链淀粉-三[3,5-二甲基氨基甲酸酯]衍生物(Chiralpak AD)手性色谱柱(4.6 mm×250 mm),流动相:正己烷-无水乙醇-三氟乙酸(90∶10∶0.1),流速0.5 ml/min,检测波长:239 nm。
结果:在建立的手性分离方法下,氟伐他汀消旋体在20 μmol/L~300 μmol/L浓度范围内线性关系良好,两个对映异构体的相关系数r2分别为0.9993、0.9997,方法回收率为(99.4±0.8)%,日内、日间精密度(RSD)均小于10%。
结论:建立的正相手性固定相高效液相色谱法分离和测定细胞裂解液中氟伐他汀对映体的方法准确、可靠,可用于体外细胞模型中氟伐他汀的立体选择性研究。

关键词: 氟伐他汀/分离和提纯,  色谱法,  高压液相/方法,  立体异构现象 
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