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微浓缩器与固相微萃取相结合用于气相色谱-质谱分析痕量挥发性有机化合物。

Integration of a micropreconcentrator with solid-phase microextraction for analysis of trace volatile organic compounds by gas chromatography-mass spectrometry.

机构信息

Department of Chemical Engineering.

Department of Chemistry, University of Louisville, Louisville, KY 40208, United States.

出版信息

J Chromatogr A. 2022 Jun 21;1673:463083. doi: 10.1016/j.chroma.2022.463083. Epub 2022 Apr 22.

Abstract

The analysis of toxic volatile organic compounds (VOCs) in environmental air is important because toxic VOCs induce adverse effects on human health. Although gas chromatography- mass spectrometry (GC-MS) is the standard instrument for analysis of trace VOCs in air, this mode of analysis requires preconcentration and cryogenic processes. The preconcentration and subsequent thermal desorption of VOCs require special instruments and a long time of processing sample that significantly limit applications of GC-MS for monitoring indoor and outdoor VOC levels. Using a microfabricated preconcentrator for VOC analysis also has the challenge of a large sample volume for concentration. Using solid-phase microextraction (SPME) for VOC analysis by GC-MS often approaches the limit of detection of the GC-MS instrument for trace VOCs in air. This work reports a simple method to integrate microfabricated preconcentrators with commercial SPME fibers in a two-stage concentration processes to achieve rapid and reliable measurement of trace VOCs in air by GC-MS. We designed and fabricated a preconcentrator with micropillars in a microfluidic chamber to support sorbents and to increase the heat transfer rate to the sorbents for rapid thermal desorption. The effects of air flow rates through the preconcentrator on VOCs adsorption and thermal desorption were optimized for increasing analytical accuracy of VOCs measurements. The integration of a micropreconcentrator with SPME enabled measurements of sub-ppb levels of benzene, toluene, ethylbenzene, and xylene (BTEX), and trichloroethylene (TCE) in environmental air by GC-MS.

摘要

分析环境空气中有毒挥发性有机化合物(VOCs)非常重要,因为有毒 VOCs 会对人类健康产生不良影响。虽然气相色谱-质谱联用仪(GC-MS)是分析空气中痕量 VOCs 的标准仪器,但这种分析模式需要预浓缩和低温过程。VOCs 的预浓缩和随后的热解吸需要特殊的仪器和长时间的样品处理,这极大地限制了 GC-MS 用于监测室内和室外 VOC 水平的应用。使用微制造的预浓缩器进行 VOC 分析也面临着需要大体积样品进行浓缩的挑战。使用固相微萃取(SPME)与 GC-MS 联用进行 VOC 分析,通常接近 GC-MS 仪器对空气中痕量 VOC 的检测限。本工作报道了一种简单的方法,即将微制造的预浓缩器与商业 SPME 纤维集成在两级浓缩过程中,以实现通过 GC-MS 快速可靠地测量空气中的痕量 VOC。我们设计并制造了一种带有微柱的微流控室中的预浓缩器,以支撑吸附剂并提高吸附剂的传热速率,以实现快速热解吸。优化了通过预浓缩器的空气流速对 VOCs 吸附和热解吸的影响,以提高 VOCs 测量的分析准确性。微预浓缩器与 SPME 的集成使我们能够通过 GC-MS 测量环境空气中的苯、甲苯、乙苯和二甲苯(BTEX)以及三氯乙烯(TCE)的亚 ppb 水平。

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