色谱

色谱 ›› 2011, Vol. 29 ›› Issue (01): 91-94.DOI: 10.3724/SP.J.1123.2011.00091

• 技术与应用 • 上一篇    

七(2,3,6-三-O-甲氧甲基)-β-环糊精的合成及其在气相色谱分离中的应用

尹明明1, 朱小波2, 刘勇良1, 钟江春3, 陈福良1*   

  1. 1. 农业部农药化学与应用重点开放实验室, 中国农业科学院植物保护研究所, 北京 100193; 2. 中国民用航空局第二研究所, 四川 成都 610041; 3. 中国农业大学理学院, 北京 100193
  • 收稿日期:2010-09-15 修回日期:2010-11-01 出版日期:2011-01-28 发布日期:2011-01-28
  • 通讯作者: 陈福良,博士,副研究员. Tel: (010)62815939

Synthesis of heptakis(2,3,6-tri-O-methoxymethyl)-β-cyclodextrin and its application in gas chromatography

YIN Mingming1, ZHU Xiaobo2, LIU Yongliang1, ZHONG Jiangchun3, CHEN Fuliang1*   

  1. 1. Key Laboratory of Pesticide Chemistry and Application Technology of Ministry of Agriculture, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, China; 2. Second Research Institute of Civil Aviation Administration of China, Chengdu 610041, China; 3. College of Science, China Agricultural University, Beijing 100193, China
  • Received:2010-09-15 Revised:2010-11-01 Online:2011-01-28 Published:2011-01-28

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摘要： 将甲氧甲基引入β-环糊精的2,3,6-位合成了新的气相色谱手性固定相七(2,3,6-三-O-甲氧甲基)-β-环糊精,并采用静态法将其涂渍在毛细管内壁制备毛细管气相色谱柱。考察了毛细管柱的柱性能和分离性能。结果表明该固定相对Grob试剂、苯的二取代位置异构体(硝基甲苯、溴甲苯、二氯苯和二甲苯)及手性化合物(2-羟基丙酸甲酯、2-羟基丙酸乙酯和2-甲磺酰基丙酸甲酯)都具有良好的分离效果。与固定相2,3,6-三-O-甲基-β-环糊精的手性分离效果对比,结果显示两种手性固定相的分离能力各异,对一些手性脂类化合物对映体的分离存在互补性。

关键词: 固定相, 环糊精衍生物, 毛细管气相色谱, 手性化合物, 位置异构体

Abstract: A new chiral stationary phase for gas chromatography, heptakis(2,3,6-tri-O-methoxymethyl)-β-cyclodextrin, was synthesized by substituting the 2,3,6-OH groups of β-cyclodextrin with methoxymethyl groups, and a coated capillary column for gas chromatography was made by coating this new stationary phase with static method. The chromatographic properties and separation abilities of the prepared stationary phase were studied. The test results showed that it possessed good separation abilities to Grob test mixture, disubstituted benzene isomers (e.g. nitrotoluenes, bromotoluenes, dichlorobenzenes, dimethylbenzenes) and some chiral compounds such as methyl 2-hydroxypropionates, ethyl 2-hydroxypropionates, methyl 2-methylsulfonylpropionates. The comparison of chiral separation results between 2,3,6-tri-O-methoxymethyl-β-cyclodextrin and 2,3,6-tri-O-methyl-β-cyclodextrin showed that the separation abilities of the two stationary phases were different and complementary to each other for some chiral ester enantiomers.

Key words: capillary gas chromatography （CGC）, chiral compounds, positional isomers, stationary phase, cyclodextrin derivatives

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