气相色谱法测定R-4-氯-3-羟基丁酸乙酯中的杂质  

Determination of impurities in Ethyl(R)-(+)-4-chloro-3-hydroxybutyrate by Gas chromatographic

作　　者：赵军霞 洪瑞梅 李慧思 孙保国 Zhao Jun-xia;Hong Rui-mei;Li Hui-si;Sun Bao-guo(Enzymaster Bioengineering Co Ltd.,Ningbo,Zhejiang 315000,China)

机构地区：[1]宁波酶赛生物工程有限公司,浙江宁波315000

出　　处：《福建分析测试》2025年第1期24-29,共6页Fujian Analysis & Testing

摘　　要：本文开发了一种能同时检测4-氯乙酰乙酸乙酯、乙酰乙酸乙酯、2-氯乙酰乙酸乙酯、4-氯乙酰乙酸甲酯、3-羟基丁酸乙酯和R-4-氯-3-羟基丁酸乙酯等六种化合物的气相色谱方法。用DB-WAX色谱柱,采用分流进样方式,氢火焰离子化检测器(FID)能够检测和分离反应体系中存在的各物质。4-氯乙酰乙酸乙酯、乙酰乙酸乙酯、2-氯乙酰乙酸乙酯、4-氯乙酰乙酸甲酯、3-羟基丁酸乙酯和R-4-氯-3-羟基丁酸乙酯分别在4.497~29.98μg/mL、3.001~30.01μg/mL、3.021~30.21μg/mL、1.517~22.76μg/mL、1.577~23.66μg/mL和1.001-12006.9μg/mL范围内呈线性关系,相关系数分别0.9998、0.9991、0.9990、0.9990、0.9996和0.9999。4-氯乙酰乙酸乙酯、乙酰乙酸乙酯、2-氯乙酰乙酸乙酯、4-氯乙酰乙酸甲酯和3-羟基丁酸乙酯的回收率分别为98.51%~98.93%、98.94%~102.93%、99.35%~103.31%、95.23%~99.58%和97.23%~98.79%。本方法可用于酶法合成R-4-氯-3-羟基丁酸乙酯反应过程中杂质研究和最终产品R-4-氯-3-羟基丁酸乙酯的杂质检测。本方法操作简单、稳定性、灵敏度和准确性都很好。In this paper,a gas chromatography method was established for simultaneous detection of six compounds,includ⁃ing ethyl 4-chloroacetoacetate,ethyl acetoacetate,ethyl 2-chloroacetoacetate,methyl 4-chloro-3-oxo-butanoate,ethyl 3-hydroxybutyrate and ethyl(R)-(+)-4-chloro-3-hydroxybutyrate.Using DB-WAX column,split sampling,and FID as de⁃tector can detect and separate the substances in the reaction system.Ethyl 4-chloroacetoacetate,ethyl acetoacetate,ethyl 2-chloroacetoacetate,methyl 4-chloro-3-oxo-butanoate,ethyl 3-hydroxybutyrate and ethyl(R)-(+)-4-chloro-3-hydroxy⁃butyrate had a good linear relationship in the range of 4.497-29.98μg/mL,3.001-30.01μg/mL,3.021-30.21μg/mL,1.517-22.76μg/mL,1.577-23.655μg/mL and 1.001-12006.9μg/mL,the correlation coefficients were 0.9998、0.9991、0.9990、0.9990、0.9996 and 0.9999,respectively.The average recovery rate of ethyl 4-chloroacetoacetate,ethyl acetoace⁃tate,ethyl 2-chloroacetoacetate,methyl 4-chloro-3-oxo-butanoate and ethyl 3-hydroxybutyrate were 98.51%-98.93%,98.94%-102.93%,99.35%-103.31%,95.23%-99.58%and 97.23%-98.79%,respectively.The method can be used to study the impurities in the enzymatic synthesis of ethyl(R)-(+)-4-chloro-3-hydroxybutyrate and to detect the impurities in the final product of ethyl(R)-(+)-4-chloro-3-hydroxybutyrate.This method has the advantages of simple operation,good stability,sensitivity and accuracy.

关 键 词：气相色谱法 R-4-氯-3-羟基丁酸乙酯 杂质 

分 类 号：O657.71[理学—分析化学]