Use of a Novel Sol–Gel Dibenzo-18-Crown-6 Solid-Phase Microextraction Fiber and a New Derivatizing Reagent for Determination of Aliphatic Amines in Lake Water and Human Urine

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• 作者：Lingshuang Cai ; Yuanyuan Zhao ; Shuling Gong ; Li Dong and Caiying Wu
• 关键词：Gas chromatography Solid ; phase microextraction Dibenzo ; 18 ; crown ; 6 ; coated fibres Tetrafluorobenzoic acid ; N ; hydroxysuccinimide ester Aliphatic amine derivatives
• 刊名：Chromatographia
• 出版年：2003
• 出版时间：November 2003
• 年：2003
• 卷：58
• 期：9-10
• 页码：615-621
• 全文大小：293 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

Dibenzo-18-crown-6 as a novel coating for solid phase microextraction (SPME) fibers has been prepared by sol–gel technology. The performance of the coating is stable at high temperature (350 °C) and the coating has a long lifetime (it can be used more than 150 times). The extraction properties of the new coating for derivatized aliphatic amines such as methylamine, dimethylamine, ethylamine, propylamine, butylamine, pentylamine, and hexylamine were investigated. Compared with commercial 100 m PDMS and 85 m PA fibers the sol–gel dibenzo-18-crown-6 coating is more sensitive and selective for derivatized aliphatic amines. A new derivatizing reagent, tetrafluorobenzoic acid N-hydroxysuccinimide ester (TFBza-suc) was synthesized for derivatization of aliphatic amines. In pH 8.3 H₃BO₃–Na₂B₄O₇ buffer at 40 °C in a water bath the derivatization reaction is complete within 15 min and excess reagent need not be removed, which greatly simplifies sample preparation. The selectivity and sensitivity of this method for determination of aliphatic amines in lake water and urine can be significantly improved by coupling derivatization with SPME during sampling. The calibration plot was highly linear throughout the concentration range 0.1 to 1000 g L–1. Method detection limits were below 0.05 g L–1 for GC–FID. The reproducibility of the method was less than 6% RSD. Lake water and urine samples were analyzed.