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采用顶空固相微萃取和气相色谱-质谱法分析水中的线性和环状甲基硅氧烷。

Analysis of linear and cyclic methylsiloxanes in water by headspace-solid phase microextraction and gas chromatography-mass spectrometry.

机构信息

Analytical Chemistry Department, University of Barcelona, Avda. Diagonal 647, 08028 Barcelona, Spain.

出版信息

Talanta. 2012 Jan 30;89:63-9. doi: 10.1016/j.talanta.2011.11.058. Epub 2011 Nov 26.

Abstract

This paper proposes a new method for the analysis of linear and cyclic methylsiloxanes in water samples based on headspace-solid phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). The extraction efficiency of four commercially available SPME-fibres was evaluated and it was found that a 65 μm polydimethylsiloxane/divinylbenzene (PDMS/DVB) coating was the most suitable for the extraction of siloxanes. The method provided good linearity (r>0.999) and precision (RSD % <17%), and low limits of quantification ranging from 0.01 to 0.74 ng L(-1) for linear siloxanes and between 18 and 34 ng L(-1) for cyclic siloxanes. The HS-SPME-GC-MS method was applied to the analysis of linear and cyclic siloxanes in river waters from Catalonia (NE, Spain) and the results showed concentrations of linear and cyclic siloxanes ranging from 0.09 to 3.94 ng L(-1) and 22.2 to 58.5 ng L(-1), respectively.

摘要

本文提出了一种基于顶空固相微萃取(HS-SPME)与气相色谱-质谱联用(GC-MS)分析水样中环状和线状甲基硅氧烷的新方法。评估了四种市售 SPME 纤维的萃取效率,发现 65μm 聚二甲基硅氧烷/二乙烯基苯(PDMS/DVB)涂层最适合硅氧烷的萃取。该方法具有良好的线性(r>0.999)和精密度(RSD%<17%),线性硅氧烷的定量下限范围为 0.01-0.74ng L(-1),环状硅氧烷的定量下限范围为 18-34ng L(-1)。HS-SPME-GC-MS 方法应用于分析来自西班牙东北部加泰罗尼亚(Catalonia)的河水,结果表明线性和环状硅氧烷的浓度分别为 0.09-3.94ng L(-1)和 22.2-58.5ng L(-1)。

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