色谱

色谱 ›› 2014, Vol. 32 ›› Issue (10): 1117-1123.DOI: 10.3724/SP.J.1123.2014.09010

• 研究论文 • 上一篇    下一篇

纤维素/聚硅氧烷离子液体混合气相色谱固定相的制备

陈刚1, 赵晓洁2, 邢钧2, 姚玉华3, 郑京京3   

  1. 1. 广东电网公司电力科学研究院, 广东 广州 510080;
    2. 生物医学分析化学教育部重点实验室, 武汉大学化学与分子科学学院, 湖北 武汉 430072;
    3. 武汉理工大学化工学院, 湖北 武汉 430079
  • 收稿日期:2014-09-05 出版日期:2014-10-08 发布日期:2014-09-29
  • 通讯作者: 郑京京，E-mail：zjj2937@sohu.com

Preparation of mixed stationary phase of cellulose and polysiloxane ionic liquid for gas chromatography

CHEN Gang1, ZHAO Xiaojie2, XING Jun2, YAO Yuhua3, ZHENG Jingjing3   

  1. 1. Electric Power Research Institute of Guangdong Power Grid Corporation, Guangzhou 510080, China;
    2. Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, China;
    3. College of Chemical Engineering, Wuhan University of Technology, Wuhan 430079, China
  • Received:2014-09-05 Online:2014-10-08 Published:2014-09-29

PDF

249

被引次数

2

摘要：

纤维素是液相色谱中应用十分广泛的一类固定相，可是由于涂渍性能不佳，纤维素在气相色谱中的应用鲜有报道。本论文首先通过酯化反应合成了脂溶性较好的三醋酸纤维素（CTA），然后与自制的聚硅氧烷离子液体（PIL-C12-NTf2）混配，制备了含纤维素的气相色谱固定相（CTA@PIL-C12-NTf2），并涂渍了毛细管柱。其柱效为3165 plates/m（110 ℃，萘，k=4.95）。麦氏常数及溶剂化参数模型的测试结果证明，该固定相属中强极性固定相，主要作用力是氢键碱性作用和偶极作用。值得注意的是，引入纤维素可明显改善三取代芳香化合物位置异构体及壬烷（C9）同分异构体的分离选择性。此外，该固定相对正构烷烃、醇、脂肪酸酯及邻苯二甲酸酯等也具有良好的分离选择性。该研究不仅初步展现了纤维素在分离选择性上的特点，而且也为探索纤维素衍生物在气相色谱中的应用提供了一条新的途径。

关键词: 固定相, 离子液体, 气相色谱, 三醋酸纤维素

Abstract:

Cellulose has been widely used to synthesize chiral stationary phases for liquid chromatography, but it is still absent in the family of stationary phases of gas chromatography due to its poor film-forming property. Based on the unique dissolution characteristic, ionic liquids provide a great chance to solve this problem. In this paper, cellulose triacetate (CTA) was synthesized, and then mixed with the home-made polysiloxane ionic liquid (PIL-C12-NTf2) to produce a novel mixed stationary phase (CTA@PIL-C12-NTf2). After that, it was used to prepare a capillary column for gas chromatography. The column efficiency was measured to be 3165 plates/m (110 ℃, naphthalene, k=4.95), demonstrating the excellent film-forming capability of this stationary phase, and then the solvation parameter model was employed to find out the interaction parameters of CTA@PIL-C12-NTf2. In the aspect of selectivity, CTA was firstly demonstrated to be able to improve the resolutions of tri-substituted aromatic positional isomers and the six isomers of nonane (C9). Moreover, some mixtures of representative chemicals like di-substituted aromatic positional isomers, n-alkanes, alcohols, aliphatic esters and phthalates can also be separated well on CTA@PIL-C12-NTf2. This work proposed a novel way for the application of cellulose modified stationary phase of gas chromatography, and revealed some features of this stationary phase in selectivity resulting from cellulose.

Key words: cellulose triacetate (CTA), gas chromatography (GC), ionic liquids (IL), stationary phase

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