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

作　　者：王东武 王西宁 丰梅君 宋莹雪 

机构地区：[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

出　　处：《分析测试学报》2014年第10期1123-1128,共6页Journal of Instrumental Analysis

摘　　要：以手性填料色谱柱为固定相，建立了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的高效液相色谱法。分别以Daicel CHlRALPAK AD-H手性色谱柱、Daicel CHlRALCEL（R） OJ-H手性色谱柱、研创SCDP52546手性色谱柱、研创RC-OD52546手性色谱柱为分离柱，进行色谱柱筛选，并考察了不同检测波长、柱温及流动相体系对对映异构体和非对映异构体分离检测的影响。优化后的色谱条件为：以Daicel CHlRALPAK AD-H手性色谱柱为分离柱，正己烷-乙醇-二乙胺（900：100：1）为流动相；检测波长为220 nm；流速为1 mL/min；柱温为30℃。该色谱条件专属性良好（分离度≥2.0）；精密度良好（ RSD≤2.0％）；对映异构体、非对映异构体Ⅰ、非对映异构体Ⅱ分别在0.2405-10.8225，0.1868-8.4060，0.1961-8.8245μg/mL范围内线性关系良好（ r≥0.999）；检出限为0.06225-0.08013μg/mL，定量下限为0.1868-0.2405μg/mL；加标回收率为94.4％-95.7％，相对标准偏差为2.5％-3.1％。该方法简便、有效，可用于生产中琥珀酸索利那新原料药中对映异构体和非对映异构体的含量检测。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 ＆amp; Cretivity SCDP52546 column and Research＆amp;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：DaicellCHlRALPAKAD-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 

分 类 号：O657.760.72[理学—分析化学]