首页|柱前衍生气相色谱法分离手性二醇类化合物

柱前衍生气相色谱法分离手性二醇类化合物

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本文建立了柱前衍生气相色谱法分离1,3-丁二醇、2,3-丁二醇、2,5-己二醇和3,6-辛二醇4种二醇类化合物的手性分离方法.分别使用N-甲基-N-(三甲基硅烷)三氟乙酰胺和三氟乙酸酐为衍生剂与二醇化合物反应,生成相应的衍生物,用CP-Chirasil-Dex CB色谱柱分离二醇对映体,采用分流进样方式,检测器为氢火焰离子化检测器(FID).在选定的色谱条件下,四种手性化合物分别在2.50~8×103µg/mL、1.30~8×103µg/mL、3.5~1×104µg/mL、5~1×104µg/mL范围内呈线性关系,相关系数分别为0.9994、0.9997、0.9990和0.9971,手性分离度均达到2以上,检测限分别为0.8µg/mL、0.4µg/mL、1.8µg/mL、2.5µg/mL.该方法适用于生物酶催化反应所生成的(2R,3R)-2,3-丁二醇、(R)-1,3-丁二醇、(2S,5S)-2,5-丁二醇和(3S,6S)-3,6-辛二醇的检测以及酶促反应过程的监控.
Pre-column Derivatization GC Method of Chiral Diols
A method of the chiral separation of 1,3-butanediol,2,5-hexadiol,3,6-octanediol and 3,6-octanediol enantio-mers via derivatization-capillary column gas chromatography was established and validated.The diol enantiomers were de-rivatized with N-methyl-n-(trimethylsilane)trifluoroacetamide or trifluoroacetic anhydride and then were separated by CP-Chirasil-Dex CB column,split sampling,and FID as detector.The linearity of the methods were proven well with the correlation coefficients were 0.9994,0.9997,0.9990,and 0.9971,as well as the detection ranges of 2.50-8×103 µg/mL,1.30-8×103µg/mL,3.5-1×104µg/mL and 5-1×104µg/mL.All the resolution factors of enantiomers separation were above 2.The detection limits of 4 analytes were 0.8µg/mL,0.4µg/mL,1.8µg/mL,and 2.5µg/mL,respectively.The method is ap-plied in the determination of(R)-1,3-butanediol,(2R,3R)-2,3-butanediol,(2S,5S)-2,5-hexanediol and(3S,6S)-3,6-octanediol which were produced by enzymatic reaction and the enzymatic reaction monitoring as well.

chiral separation1,3-butanediol2,3-butanediol2,5-hexanediol3,6-octanediol

洪瑞梅、杨欣航、赵军霞、陈承、孙保国

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宁波酶赛生物工程有限公司,浙江 宁波 315000

手性分离 1,3-丁二醇 2,3-丁二醇 2,5-己二醇 3,6-辛二醇

2024

福建分析测试
福建省测试技术研究所

福建分析测试

影响因子:0.365
ISSN:1009-8143
年,卷(期):2024.33(1)
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