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基于聚硅氧烷的萃取方法与大体积进样-气相色谱-质谱联用技术在水样中有机化合物分析中的应用。

Application of a polysiloxane-based extraction method combined with large volume injection-gas chromatography-mass spectrometry of organic compounds in water samples.

作者信息

Schellin Manuela, Popp Peter

机构信息

Department of Analytical Chemistry, Helmholtz Centre for Environmental Research-UFZ, Permoserstrasse 15, 04318 Leipzig, Germany.

出版信息

J Chromatogr A. 2007 Jun 8;1152(1-2):175-83. doi: 10.1016/j.chroma.2007.01.087. Epub 2007 Jan 30.

Abstract

This work describes a novel, simple, and inexpensive approach for an absorptive extraction of organic contaminants from aqueous samples applying polysiloxane tubes. After the extraction, the tubes were desorbed with 200 microL of an organic solvent and 50 microL of the extract were transferred via large volume injection (LVI) into a gas chromatography-mass spectrometry system (GC-MS). Fourteen organic compounds covering a broad range in polarity with log K(o/w)-values between 2.6 (atrazine) and 7 (polychlorinated biphenyl 138, PCB 138) were chosen as model compounds. The experimental parameters affecting the efficiency of the process such as desorption solvents, the addition of salt and pH-change, the extraction and desorption time were carefully optimised. The recoveries were compared with theoretical values. The limits of detection (LODs) were in the range of 0.5-5 ng/L and the precision was 7-15%. The method was successfully applied to the analysis of a contaminated river water sample.

摘要

这项工作描述了一种新颖、简单且廉价的方法,用于使用聚硅氧烷管从水性样品中吸收萃取有机污染物。萃取后,用200微升有机溶剂对管进行解吸,并通过大体积进样(LVI)将50微升萃取物转移至气相色谱 - 质谱系统(GC - MS)中。选择了14种极性范围广泛、log K(o/w)值在2.6(阿特拉津)至7(多氯联苯138,PCB 138)之间的有机化合物作为模型化合物。仔细优化了影响该过程效率的实验参数,如解吸溶剂、盐的添加和pH变化、萃取和解吸时间。将回收率与理论值进行了比较。检测限(LOD)在0.5 - 5 ng/L范围内,精密度为7 - 15%。该方法成功应用于受污染河水样品的分析。

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