色谱

色谱

• 研究论文 • 上一篇    下一篇

应用于全氟辛烷磺酸萃取富集的全氟癸基修饰毛细管硅胶整体柱的制备及应用

黄科1, 周乃元2, 陈波1*   

  1. 1. 湖南师范大学化学生物学及中药分析教育部重点实验室
    2. 湖南师范大学
  • 收稿日期:2011-04-18 修回日期:2011-05-24 出版日期:2011-10-28 发布日期:2011-10-13
  • 通讯作者: 陈波,教授,主要研究方向为药物与色谱分析. Tel: (0731)88865515,
  • 基金资助:
    国家自然科学基金项目(Nos. 20927005, 20875028, 20080542003, 2008［890］)、国家“863”课题(No. 2010AA023001)和湖南省科技计划课题(Nos. 05k009, 2010TT1001).

Preparation and application of perfluorodecyl modified silica monolithic capillary column in extraction and enrichment of perfluorooctane sulfonates

HUANG Ke1, ZHOU Naiyuan2, CHEN Bo1*   

  1. 1. Key Laboratory of Chemical Biology & Traditional Chinese Medicine Research, Ministry of Education, Hunan Normal University, Changsha 410081, China; 2. China National Center for Biotechnology Development, Beijing 100036, China
  • Received:2011-04-18 Revised:2011-05-24 Online:2011-10-28 Published:2011-10-13

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摘要： 利用溶胶-凝胶法,经过烷氧基硅烷的水解、硅羟基的缩聚、凝胶化、陈化、中孔制备、干燥和表面修饰等步骤制备了全氟癸基修饰的毛细管硅胶整体柱。采用该整体柱对全氟辛烷磺酸(PFOS)进行萃取富集,考察其富集特性和效率,并与传统的C18毛细管硅胶整体柱进行对比。结果表明,全氟癸基修饰毛细管硅胶整体柱(15 cm×75 μm)对PFOS具有更高的吸附量和更好的富集选择性,其平均吸附量可以达到75 ng；样品中PFOS的质量浓度为0.25 mg/L时,富集倍数平均可以达到29倍。此全氟癸基修饰毛细管硅胶整体柱对PFOS具有良好的萃取富集性能,可用于水质中痕量PFOS的萃取富集。

关键词: 富集, 固相萃取, 全氟癸基修饰毛细管硅胶整体柱, 全氟辛烷磺酸盐

Abstract: A perfluorodecyl modified silica monolithic capillary column has been prepared by using sol-gel method. The preparation steps included hydrolysis of alkoxy silane, fasculation of silanol, gelation, aging, meso-pore preparation, drying and surface modification. It could be used as a solid phase extraction (SPE) microcolumn for extraction and enrichment of perfluorooctane sulfonate (PFOS). The enrichment characteristics and efficiency of the perfluorodecyl modified monolithic silica capillary column has been investigated and compared with C18 silica monolithic capillary column. The results indicated that the perfluorodecyl modified silica monolithic capillary column (15 cm×75 μm) had a higher adsorption capacity and a better enrichment selectivity for PFOS. The average adsorption capacity of the perfluorodecyl modified silica monolithic capillary column was 75 ng. And when the PFOS mass concentration in sample was 0.25 mg/L, the enrichment factor was 29-fold in average. Owing to the good performance of the perfluorodecyl modified silica monolithic capillary column, it can be used for the extraction and enrichment of trace PFOS in water to meet the requirements of water quality monitoring and analysis.

Key words: enrichment, perfluorooctane sulfonate (PFOS), solid phase extraction (SPE), perfluorodecyl modified silica monolithic capillary column