Sampling and analysis of polychlorinated biphenyls in indoor air by sorbent enrichment followed by headspace solid-phase microextraction and gas chromatography-tandem mass spectrometry

被引:26
作者
Barro, R [1 ]
Ares, S [1 ]
Garcia-Jares, C [1 ]
Llompart, M [1 ]
Cela, R [1 ]
机构
[1] Univ Santiago de Compostela, Inst Invest & Anal Alimentario, Dept Quim Analit Nutr & Bromatol, Fac Quim, E-15782 Santiago De Compostela, Spain
关键词
air analysis; polychlorinated biphenyls; solid-phase microextraction; solid-phase extraction; factorial design; chlorinated compounds;
D O I
10.1016/j.chroma.2004.12.062
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
In this study, a combination of solid-phase extraction (SPE) and solid-phase microextraction (SPME) techniques has been used to determine polychlorinated biphenyls (PCBs) in air. Using a vacuum pump, a known volume of air was pulled through a porous polymer (Tenax TA) where the target analytes were retained and then headspace SPME was carried out. The quantification was performed using gas chromatography coupled to tandem mass spectrometry. Certain factors, such as temperature and the addition of solvents to the adsorbent, were found to be very important for the transfer of the target PCBs from the Tenax to the SPME fiber. Some of these factors were studied using an experimental design strategy. Performance of the method was evaluated demonstrating that external calibration, which does not require performing the complete sampling process, was suitable. The coefficients of determination were calculated and a lack-of-fit test was run within the calibration data, demonstrating linearity of the method. Repeatability was found adequate (RSD <= 12%). Limits of detection (LODs) were found below 0.100 ng/m(3) when only 2.5 m(3) air were sampled. These LODs were low enough to check for harmful levels of PCBs in indoor air, and are well below the most restrictive limits established by countries regulations. In addition, more sensitivity could be attained by increasing the volume of air sampled (decrease in retention efficiency was not detected for sample volumes up to 25 m(3)), and/or extending the extraction time in the SPME step. (c) 2004 Elsevier B.V. All rights reserved.
引用
收藏
页码:99 / 106
页数:8
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