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气相色谱-三重四极杆串联质谱法:一种用于(超)痕量分析鱼类和鱼饲料中多类环境污染物的强大工具。

Gas chromatography-triple quadrupole tandem mass spectrometry: a powerful tool for the (ultra)trace analysis of multiclass environmental contaminants in fish and fish feed.

机构信息

Department of Food Analysis and Nutrition, Faculty of Food and Biochemical Technology, Institute of Chemical Technology, Prague, Technicka 3, 166 28, Prague 6, Czech Republic.

出版信息

Anal Bioanal Chem. 2013 Sep;405(24):7803-15. doi: 10.1007/s00216-013-7000-4. Epub 2013 May 10.

Abstract

A new method for rapid determination of 73 target organic environmental contaminants including 18 polychlorinated biphenyls, 16 organochlorinated pesticides, 14 brominated flame retardants and 25 polycyclic aromatic hydrocarbons in fish and fish feed using gas chromatography coupled with triple quadrupole tandem mass spectrometry (GC-MS/MS) was developed and validated. GC-MS/MS in electron ionization mode was shown to be a powerful tool for the (ultra)trace analysis of multiclass environmental contaminants in complex matrices, providing measurements with high selectivity and sensitivity. Another positive aspect characterizing the newly developed method is a substantial simplification of the sample preparation, which was achieved by an ethyl acetate QuEChERS (quick, easy, cheap, effective, rugged and safe) based extraction followed by silica minicolumn clean-up. With use of this sample preparation approach the sample laboratory throughput was increased not only because six samples may be prepared in approximately 1 h, but also because all the above-mentioned groups of contaminants can be determined in a single GC-MS/MS run. Under the optimized conditions, the recoveries of all target analytes in both matrices were within the range from 70 to 120% and the repeatabilities were 20% or less. The method quantification limits were in the range from 0.005 to 1 μg kg(-1) and from 0.05 to 10 μg kg(-1) for fish muscle tissue and fish feed, respectively. The developed method was successfully applied to the determination of halogenated persistent organic pollutants and polycyclic aromatic hydrocarbons in fish and fish feed samples.

摘要

建立并验证了一种利用气相色谱-三重四极杆串联质谱(GC-MS/MS)快速测定鱼肉和鱼饲料中 73 种目标有机环境污染物(包括 18 种多氯联苯、16 种有机氯农药、14 种溴代阻燃剂和 25 种多环芳烃)的新方法。电子电离模式下的 GC-MS/MS 被证明是一种强大的工具,可用于在复杂基质中对多类环境污染物进行(超)痕量分析,提供具有高选择性和灵敏度的测量结果。该新方法的另一个积极特点是样品制备的大幅简化,这是通过乙酸乙酯 QuEChERS(快速、简单、廉价、有效、耐用和安全)提取,然后用硅胶小柱净化来实现的。使用这种样品制备方法,不仅可以在大约 1 小时内制备 6 个样品,而且可以在单个 GC-MS/MS 运行中同时测定上述所有污染物组,从而提高了样品实验室的通量。在优化条件下,两种基质中所有目标分析物的回收率均在 70%至 120%范围内,重复性为 20%或更低。该方法的定量限在鱼肉组织和鱼饲料中分别为 0.005 至 1μgkg-1 和 0.05 至 10μgkg-1。所建立的方法成功应用于鱼肉和鱼饲料样品中卤代持久性有机污染物和多环芳烃的测定。

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