| 手性医药中间体4-氯-3-羟基丁酸乙酯的气相色谱分析 |
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| 引用本文： | 韦善怀,;徐燕,;韦志明,;黄平,;黄科润,;穆允玲,;莫友彬.手性医药中间体4-氯-3-羟基丁酸乙酯的气相色谱分析[J].化工技术与开发,2014(7):45-47. |
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| 作者姓名： | 韦善怀 ;徐燕 ;韦志明 ;黄平 ;黄科润 ;穆允玲 ;莫友彬 |
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| 作者单位： | [1]广西化工研究院,广西南宁530001; [2]广西科技情报研究所,广西南宁530004 |
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| 基金项目： | 广西自然科学基金项目（2011GXNSFA018052） |
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| 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。
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| 关 键 词： | 气相色谱法 内标法 -氯乙酰乙酸乙酯 手性-氯--羟基丁酸乙酯 |
Determination of Chiral Pharmaceutical Intermediates Ethyl 4-Chloro-3-hydroxybutyrate by Gas Chromatographic |
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| Affiliation: | WEI Shan-huai, XU Yan, WEI Zhi-ming, HUANG Pimg, HUANG Ke-run, MU Yun-ling, MO You-bin (1. Guangxi Research Institute of Chemical Industry, Nanning 530001, China; 2. Guangxi Institute of Science and Technology Information, Nanning 530022, China) |
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| Abstract: | A gas chromatographic method for the determination of pharmaceutical intermediates chiral ethyl 4-chloro-3-hydroxybu-tyrate 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%. |
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| Keywords: | gas chromatography internal standard method ethyl 4-chloroacetoacetate chiral ethyl 4-chloro-3-hydroxybutyrate |
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