Development of a Sol-Gel Procedure for Preparation of a Diglycidyloxycalix[4]arene Solid-Phase Microextraction Fiber with Enhanced Extraction Efficiency

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• 作者：Xiujuan Li ; Shuling Gong and Zhaorui Zeng
• 关键词：Gas chromatography ; Solid ; phase microextraction ; Calixarene ; coated fibers ; Polycyclic aromatic hydrocarbons ; amines ; and phenols ; Sol ; gel procedure
• 刊名：Chromatographia
• 出版年：2005
• 出版时间：November 2005
• 年：2005
• 卷：62
• 期：9-10
• 页码：519-525
• 全文大小：368 KB
• 刊物类别：Chemistry and Materials Science
• 刊物主题：Chemistry
  Analytical Chemistry
  Organic Chemistry
  Pharmacy
  Biochemistry
  Plant Sciences
  Measurement Science and Instrumentation
  
• 出版者：Vieweg Verlag
• ISSN：1612-1112

文摘

5,11,17,23-Tetra-tert-butyl-25,27-dihydroxy-26,28-diglycidyloxycalix[4]arene (diglycidyloxy-C[4]) has been synthesized and used for preparation of a sol-gel solid-phase microextraction fiber with enhanced extraction efficiency. The sol-gel procedure was developed using a sol solution containing diglycidyloxy-C[4] as organic component and both tetraethoxysilane and 3-aminopropyltriethoxysilane (KH-550) as precursors. No additional catalysts were used and no centrifugation was performed. Diglycidyloxy-C[4] was highly chemically reactive toward KH-550 even at room temperature, which increased the calixarene content of the coating, simplified the sol-gel procedure, reduced the sol-gel reaction time, enhanced the polarity of the coating, and improved extraction performance. The sol-gel mixture also had very good coating properties and was highly uniformly distributed on the surface of the fiber; because of these characteristics several fibers could be prepared from one sol-gel solution. Efficient extraction of trace analytes (μg L?1 levels) from aqueous samples was accomplished using this kind of new fiber. Very low detection limits (ng L?1 level) were achieved for most polar (aromatic amines and phenols) and nonpolar (polycyclic aromatic hydrocarbons) aromatic compounds by SPME followed by gas chromatography with flame ionization detection. The new coating had excellent solvent and thermal (350 °C) stability. Lifespan was also good—a fiber could be used more than 300 times in headspace SPME without substantial changes in the properties of the coating.