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手性医药中间体4-氯-3-羟基丁酸乙酯的气相色谱分析
Determination of Chiral Pharmaceutical Intermediates Ethyl 4-Chloro-3-hydroxybutyrate by Gas Chromatographic
【摘要】 采用气相色谱法测定4-氯乙酰乙酸乙酯不对称催化还原手性4-氯-3-羟基丁酸乙酯反应体系中相关组分的含量。选择手性色谱柱及1,3-丁二醇内标物为色谱条件,在此条件下各种物质能很好地分离,该方法的检出限为10.24~19.56 mg·L-1,相对标准偏差为0.42%~0.68%,加标回收率为97.7%~101.3%,其精密度和准确度均能满足常规分析要求。
【Abstract】 A gas chromatographic method for the determination of pharmaceutical intermediates chiral ethyl 4-chloro-3-hydroxybutyrate from ethyl 4-chloroacetoacetate by the asymmetric hydrogenation was described.Chiral capillary column and 1,3-butanediol as internal standard were chosen as chromatographic conditions,in which all components could be separated and determined.The detection limit was less than 20mg/L,the RSD was 0.42%~0.68% and the recovery was 97.7%~101.3%.
【关键词】 气相色谱法；
内标法；
4-氯乙酰乙酸乙酯；
手性4-氯-3-羟基丁酸乙酯；
【Key words】 gas chromatography； internal standard method； ethyl 4-chloroacetoacetate； chiral ethyl 4-chloro-3-hydroxybutyrate；
【Key words】 gas chromatography； internal standard method； ethyl 4-chloroacetoacetate； chiral ethyl 4-chloro-3-hydroxybutyrate；
【基金】 广西自然科学基金项目(2011GXNSFA018052)
- 【文献出处】 化工技术与开发 ,Technology & Development of Chemical Industry , 编辑部邮箱 ,2014年07期
- 【分类号】R914;O657.71
- 【下载频次】269