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基于搅拌棒吸附萃取和热解吸的保留时间锁定气相色谱-质谱联用自动测定天然水和废水中合成麝香的方法。

A retention time locked gas chromatography-mass spectrometry method based on stir-bar sorptive extraction and thermal desorption for automated determination of synthetic musk fragrances in natural and wastewaters.

机构信息

Department of Analytical Chemistry, Faculty of Pharmacy, University of the Basque Country (UPV/EHU), Vitoria-Gasteiz, Spain.

出版信息

J Chromatogr A. 2011 May 20;1218(20):3048-55. doi: 10.1016/j.chroma.2011.03.012. Epub 2011 Mar 13.

Abstract

A stir-bar sorptive extraction (SBSE) method followed by automated thermal desorption (ATD) coupled to gas chromatography-mass spectrometry was optimized for determining trace levels of 18 synthetic fragrances (musks). Using the method developed a retention time locked library is created and converted to a screening database. This homebuilt database can be combined with deconvolution software for the identification of musks. A factorial design was provide to evaluate the main parameters and interactions between the factors affecting the process of SBSE. Operating with de MS-detector in the full-scan mode, high sensitivity with detection limits in the low ng L(-1) range, and good linearity and repeatability were achieved for all musks. The applicability of the method developed was tested in natural waters (surface and groundwater) and wastewater of a plant treatment (WWPT). The results obtained confirmed the usefulness of the proposed method for the determination and unequivocal identification of musks. This approach enables the developed method to be used for routine screening of environmental samples and posterior rapid quantitation of the positive samples.

摘要

搅拌棒吸附萃取(SBSE)法结合自动热解吸(ATD)与气相色谱-质谱联用,优化后可用于测定痕量的 18 种合成香料(麝香)。采用该方法建立了保留时间锁定库,并将其转化为筛选数据库。这个自建的数据库可以与解卷积软件结合使用,用于识别麝香。采用析因设计评估了影响 SBSE 过程的主要参数和因素之间的相互作用。采用全扫描模式下的 MS 检测器操作,可实现高灵敏度,检测限达到 ng/L 级,所有麝香均具有良好的线性和重复性。该方法的适用性在天然水(地表水和地下水)和工厂处理废水(WWPT)中进行了测试。所得结果证实了所提出方法在确定和明确识别麝香方面的有用性。该方法可用于环境样品的常规筛选以及阳性样品的快速定量。

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