分析测试学报Issue(10)：1123-1128,6.DOI:10.3969/j.issn.1004-4957.2014.10.005
手性固定相高效液相色谱法同时测定琥珀酸索利那新原料药中对映异构体和非对映异构体
Simultaneous Determination of Enantiomer and Diastereomers in Solifenacin Succinate Bulk Drug by High Performance Liquid Chromatography with Chiral Stationary Phase
王东武 1王西宁 1丰梅君 1宋莹雪1
作者信息
- 1. 迪沙药业集团国家认定企业技术中心质量研究院，山东 威海 264200
- 折叠
摘要
Abstract
A normal high performance liquid chromatography( HPLC)with chiral stationary phase for detection of enantiomer and diastereomers in solifenacin succinate bulk drug was developed. The sep-aration efficiencies of DaicellCHlRALPAK AD-H column,DaicellCHlRALCEL OJ-H column, Research & Cretivity SCDP52546 column and Research&Cretivity RC-OD52546 column for 4 opti-cal isomers were investigated. Various UV detection wavelengths,column temperatures and mobile phases types were also investigated. The best chromatographic conditions were as follows:column:DaicellCHlRALPAKAD-H column,mobile phase:n-haxane-ethanol-diethylamide(900 : 100: 1),UV detection wavelength:220 nm,flow rate:1 mL/min,column temperature:30 ℃. The method had a good specificity( resolution( R )≥2. 0 )and a good precision( RSD≤2. 0% , n=6 ). The calibration curves showed good linearities over the ranges of 0. 240 5-10. 822 5μg/mL for enan-tisomer,0. 186 8-8. 406 0 μg/mL for diastereoisomerⅠand 0. 196 1-8. 824 5 μg/mL for diastere-oisomerⅡ with correction coefficients more than 0. 999. The limits of detection( LODs)were in the range of 0. 062 25-0. 080 13 μg/mL and the limits of quantitation( LOQs)were 0. 186 8-0. 240 5μg/mL. The average spiked recoveries were in the range of 94. 4% -95. 7% with relative standard deviations of 2. 5% -3. 1% . The method was simple,sensitive and valid,and could satisfy the re-quirements for detection of enatiomer and diastereoisomers in solifenacin succinate drug substance.关键词
琥珀酸索利那新/高效液相色谱法/对映异构体/非对映异构体Key words
solifenacin succinate/high performance liquid chromatography(HPLC)/enantiomer/di-astereoisomer分类
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王东武,王西宁,丰梅君,宋莹雪..手性固定相高效液相色谱法同时测定琥珀酸索利那新原料药中对映异构体和非对映异构体[J].分析测试学报,2014,(10):1123-1128,6.
