色谱

色谱 ›› 2014, Vol. 32 ›› Issue (12): 1385-1389.DOI: 10.3724/SP.J.1123.2014.09001

• 研究论文 • 上一篇    下一篇

气相色谱-质谱/选择离子监测法用于苯乙烯不对称环氧化反应的筛选

牟瑶1, 韦思平1, 徐敏3, 陈平1, 王钦1, 杜曦2   

  1. 1. 泸州医学院药学院, 四川 泸州 646000;
    2. 泸州医学院基础医学院, 四川 泸州 646000;
    3. 成都理工大学材料与化学化工学院, 四川 成都 610059
  • 收稿日期:2014-09-01 出版日期:2014-12-08 发布日期:2014-11-28
  • 通讯作者: 王钦,E-mail:dx.d@163.com;杜曦,E-mail:wq_ring@hotmail.com
  • 基金资助:

    Sichuan Province Education Department Project (13ZB0263,13ZA0232); Luzhou City Government Project (2011-42).

Gas chromatography-mass spectrometry/selected ion monitoring for screening asymmetric epoxidation of styrene

MU Yao1, WEI Siping1, XU Min3, CHEN Ping1, WANG Qin1, DU Xi2   

  1. 1. School of Pharmaceutical Sciences, Luzhou Medical College, Luzhou 646000, China;
    2. School of Basic Medical Sciences, Luzhou Medical College, Luzhou 646000, China;
    3. College of Material and Chemistry Engineering, Chengdu University of Technology, Chengdu 610059, China
  • Received:2014-09-01 Online:2014-12-08 Published:2014-11-28

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摘要：

建立了苯乙烯不对称环氧化反应的气相色谱-质谱/选择离子监测(GC-MS/SIM)筛选方法。以乙苯为内标,利用GC-MS/SIM对苯乙烯环氧化反应样品进行分析,在选定的分析条件下完全分离并准确测定了苯乙烯和环氧苯乙烷对映异构体的含量,同时利用该方法对苯乙烯环氧化反应的正交试验进行了评估。该方法具有以下优点:高精密度(以RSD表示的精密度为1.2%~5.2%, n=5)、良好的线性关系(苯乙烯、(R)-环氧苯乙烷和(S)-环氧苯乙烷标准曲线的相关系数分别为0.9997、0.9932和0.9963)、低定量限(苯乙烯、(R)-环氧苯乙烷和(S)-环氧苯乙烷的定量限分别为1.3、1.1和0.7 mg/L)以及合理的回收率(98.2%~108.2%)。该方法为苯乙烯及其同系物的不对称环氧化反应提供了一种新的分析测定途径。

关键词: 苯乙烯, 环氧苯乙烷对映异构体, 气相色谱-质谱/选择离子监测, 正交试验

Abstract:

A screening method by gas chromatography-mass spectrometry (GC-MS) with selected ion monitoring (SIM) has been developed for asymmetric epoxidation of styrene. All samples were analyzed by GC-MS with the mode of SIM by using ethylbenzene as the internal standard, by which styrene and styrene epoxide enantiomers were completely separated and their concentrations were accurately determined. Furthermore, this method was used to evaluate the epoxidation reaction of styrene, which was optimized by orthogonal experiment. The advantages of the method are as follows: excellent precision (RSD in the range of 1.2%-5.2%, n=5), good linearity (the correlation coefficients for styrene, (R)/(S)-styrene oxide were 0.9997, 0.9932 and 0.9963, respectively), low limits of quantitation (LOQs of styrene, (R)/(S)-styrene oxide were 1.3, 1.1 and 0.7 mg/L, respectively) and reasonable recoveries (98.2%-108.2%). All in all, the method provided a new way to determine the asymmetric epoxidation mixture of styrene and its homologs.

Key words: gas chromatography-mass spectrometry/selected ion monitoring (GC-MS/SIM), orthogonal experiment, styrene, styrene oxide enantiomers

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