化学学报 ›› 2008, Vol. 66 ›› Issue (12): 1465-1469. 上一篇    下一篇

研究论文

三苄基杯[6]芳烃固相微萃取复合涂层的研制及其应用

张廉奉a,b 朱铭立b 李秀娟b 李海兵c 曾昭睿*,b   

  1. (a南阳师范学院化学系 南阳 473061)
    (b武汉大学化学与分子科学学院 武汉 430072)
    (c华中师范大学化学学院农药与化学生物学教育部重点实验室 武汉 430079)
  • 投稿日期:2007-06-20 修回日期:2007-11-20 发布日期:2008-06-28
  • 通讯作者: 曾昭睿

Preparation and Application of Calix[6]arene Multiple Coatings to Solid-phase Microextraction

ZHANG, Lian-Feng a,b ZHU, Ming-Li b LI, Xiu-Juan b LI, Hai-Bing c ZENG, Zhao-Rui *,b   

  1. (a Department of Chemistry, Nanyang Normal University, Nanyang 473061)
    (b College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072)
    (c Key Laboratory of Pesticide and Chemical Biology, Ministry of Education, College of Chemistry,
    Central China Normal University, Wuhan 430079)
  • Received:2007-06-20 Revised:2007-11-20 Published:2008-06-28
  • Contact: ZENG, Zhao-Rui

采用溶胶-凝胶方法制备了三苄基杯[6]芳烃/羟基硅油(C[6]/OH-TSO)固相微萃取(SPME)探头, 通过对多环芳烃和酞酸酯(PAEs)的分析考察了新型C[6]/OH-TSO探头的性能. 结果表明: 杯[6]芳烃SPME探头对这些非极性和弱极性的芳香化合物有很好的萃取效果和选择性, 具有耐高温、使用寿命长等特点. 建立了SPME与气相色谱-氢火焰(GC-FID)联用测定化妆品中PAEs的方法. 该方法检测限低, 重现性好(RSD<9%), 线性范围宽(2~3个数量级). 回收率在83.42%~98.85%之间.

关键词: 溶胶-凝胶, 三苄基杯[6]芳烃, 固相微萃取, 酞酸酯, 多环芳烃, 化妆品

A novel solid-phase microextraction fiber coated with calix[6]arene/hydroxyl-terminated silicone oil (C[6]/OH-TSO) was prepared with a sol-gel technology and investigated by analysis of polycyclic aromatic hydrocarbons and phthalates. The fiber exhibits not only desirable thermal stability and long lifespan, but also high extraction efficiency towards these nonpolar and moderately polar aromatic analytes. The new fiber was applied to headspace solid-phase microextraction of phthalates in cosmetics by gas chromatography with a flame ionization detector. The method showed linear response over two to three orders of magnitude with correlation coefficients (r) better than 0.997, and limits of detection ranged between 0.016 and 0.061 μg/L. The relative standard deviation values obtained were <9% and recovery rates varied from 83.42% to 98.85%.

Key words: sol-gel, calix[6]arene, solid-phase microextraction, phthalate, polycyclic aromatic hydrocarbon, cosmetics