首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Sampling and analysis of polychlorinated biphenyls in indoor air by sorbent enrichment followed by headspace solid-phase microextraction and gas chromatography-tandem mass spectrometry
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Sampling and analysis of polychlorinated biphenyls in indoor air by sorbent enrichment followed by headspace solid-phase microextraction and gas chromatography-tandem mass spectrometry

机译:吸附剂富集然后顶空固相微萃取和气相色谱-串联质谱法对室内空气中的多氯联苯进行采样和分析

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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.
机译:在这项研究中,固相萃取(SPE)和固相微萃取(SPME)技术的结合已用于确定空气中的多氯联苯(PCB)。使用真空泵,将已知体积的空气通过多孔聚合物(Tenax TA),保留目标分析物,然后进行顶空SPME。使用气相色谱-串联质谱法进行定量。发现某些因素(例如温度和向吸附剂中添加溶剂)对于将目标PCB从Tenax转移到SPME纤维非常重要。使用实验设计策略研究了其中一些因素。对方法的性能进行了评估,表明不需要进行完整采样过程的外部校准是合适的。计算了确定系数,并在校准数据内运行了失配测试,证明了该方法的线性。发现重复性足够(RSD <= 12%)。当仅采样2.5 m(3)空气时,发现极限(LOD)低于0.100 ng / m(3)。这些最低检测限低到足以检查室内空气中多氯联苯的有害水平,并且远低于国家法规规定的最严格的限制。此外,可以通过增加采样空气的体积(在高达25 m(3)的样品体积中未检测到保留效率的降低)和/或延长SPME步骤中的萃取时间来获得更高的灵敏度。 (c)2004 Elsevier B.V.保留所有权利。

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