神经保护剂3β,5α,6β-雄甾三醇原料药中3种非对映异构体的分离与含量测定

摘要

A GC method for the separation and determination of three diasteromers in neuroprotectant 3β,5α,6β-androstriol(YC-6) bulk drug was developed.The separation conditions such as column type,injection port temperature,column temperature and sample concentrate were optimized,and method validation was developed.The results showed that the method had a good specificity (resolution(R) ≥1.5) and a good precision(RSD≤2.0％,n =6).The calibration curve showed a good linearity over the concentration range of 6.0-30.0 iJ g/mL for YC-6.The response factors of three diasteromers were 1.59,1.32 and 1.41,respectively,and tbeir contents were detected by principal component self-comparison with calibration factor and internal standard method.The method was simple,sensitive and valid,and was successfully applied in the analysis of diasteromers in neuroprotectant 3β,5α,6β-androstriol bulk drug.%建立了分离与测定3β,5α,6β-雄甾三醇(YC4)原料药中3种非对映异构体的气相色谱方法.进行了分离条件的优化及方法学验证.研究结果表明:该方法可对YC-6与各非对映异构体进行分离,专属性良好(分离度≥1.5),精密度高(RSD≤2.0％);YC-6在6.0～ 30.0 mg/L质量浓度范围内线性关系良好.测定了非对映异构体的响应因子(1.59,1.32和1.41),并采用加校正因子的主成分自身对照内标法以峰面积计算各非对映异构体的含量.该方法操作简便,结果准确,可用于YC-6原料中各非对映异构体的分离及含量测定.