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气流顶空液相微萃取

Gas flow headspace liquid phase microextraction.

作者信息

Yang Cui, Qiu Jinxue, Ren Chunyan, Piao Xiangfan, Li Xifeng, Wu Xue, Li Donghao

机构信息

Key Laboratory of Nature Resource of the Changbai Mountain and Functional Molecular (Yanbian University), Ministry of Education, Park Road 977, Yanji City, Jilin Province 133002, China.

出版信息

J Chromatogr A. 2009 Nov 6;1216(45):7694-9. doi: 10.1016/j.chroma.2009.09.039. Epub 2009 Sep 20.

Abstract

There is a trend towards the use of enrichment techniques such as microextraction in the analysis of trace chemicals. Based on the theory of ideal gases, theory of gas chromatography and the original headspace liquid phase microextraction (HS-LPME) technique, a simple gas flow headspace liquid phase microextraction (GF-HS-LPME) technique has been developed, where the extracting gas phase volume is increased using a gas flow. The system is an open system, where an inert gas containing the target compounds flows continuously through a special gas outlet channel (D=1.8mm), and the target compounds are trapped on a solvent microdrop (2.4 microL) hanging on the microsyringe tip, as a result, a high enrichment factor is obtained. The parameters affecting the enrichment factor, such as the gas flow rate, the position of the microdrop, the diameter of the gas outlet channel, the temperatures of the extracting solvent and of the sample, and the extraction time, were systematically optimized for four types of polycyclic aromatic hydrocarbons. The results were compared with results obtained from HS-LPME. Under the optimized conditions (where the extraction time and the volume of the extracting sample vial were fixed at 20min and 10mL, respectively), detection limits (S/N=3) were approximately a factor of 4 lower than those for the original HS-LPME technique. The method was validated by comparison of the GF-HS-LPME and HS-LPME techniques using data for PAHs from environmental sediment samples.

摘要

在痕量化学物质分析中,存在着使用诸如微萃取等富集技术的趋势。基于理想气体理论、气相色谱理论以及原始的顶空液相微萃取(HS-LPME)技术,开发了一种简单的气流顶空液相微萃取(GF-HS-LPME)技术,其中利用气流增加萃取气相体积。该系统是一个开放系统,含有目标化合物的惰性气体持续通过一个特殊的气体出口通道(内径 = 1.8mm)流动,目标化合物被捕集在挂在微量注射器尖端的溶剂微滴(2.4微升)上,从而获得高富集因子。针对四种多环芳烃,系统地优化了影响富集因子的参数,如气流速率、微滴位置、气体出口通道直径、萃取溶剂和样品的温度以及萃取时间。将结果与HS-LPME获得的结果进行了比较。在优化条件下(萃取时间和萃取样品瓶体积分别固定为20分钟和10毫升),检测限(S/N = 3)比原始HS-LPME技术低约4倍。通过比较GF-HS-LPME和HS-LPME技术对环境沉积物样品中多环芳烃的数据,验证了该方法。

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