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建立超高效液相色谱-串联质谱法分析鱼肉及脂肪食品中全氟化合物。

Development of an ultraperformance liquid chromatography-tandem mass spectrometry method for the analysis of perfluorinated compounds in fish and Fatty food.

机构信息

Food Research Laboratory, Food and Environmental Hygiene Department, 4/F Public Health Laboratory Centre, 382 Nam Cheong Street, Hong Kong SAR, China.

出版信息

J Agric Food Chem. 2014 Jun 25;62(25):5805-11. doi: 10.1021/jf502326h. Epub 2014 Jun 12.

DOI:10.1021/jf502326h
PMID:24901300
Abstract

This paper reports the development of a method for the quantitative analysis of perfluorinated compounds (PFCs), including C6-C14 perfluorinated carboxylic acids (PFCAs) and C4-C12 perfluorinated sulfonates (PFSAs), in fish and fatty foods by ultraperformance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS) in which the UPLC was equipped a PFC Analysis Kit to eliminate background contamination. Rapid baseline separation was achieved for 17 PFCs within 12 min, and PFCs were well-resolved from potential interferences from taurodeoxycholic acid and branched isomers of PFCs. The method was validated according to Commission Regulation 2002/657/EC of the European Commission with matrices including salmon, beef, egg, and butter. Average spiked recoveries, measured at concentration levels of 0.02 (method limit of quantification (MLOQ)), 0.2, and 2 μg/kg, were in the range of 68-117% with relative standard deviations below 20%. Matrix effects were evaluated and found to be correctable by internal standardization, especially for short- and long-chained PFCs. Trueness was verified against two certified reference materials. The method has also been successfully applied to the analysis of more than 200 food samples of a risk assessment study.

摘要

本研究报告开发了一种超高效液相色谱-电喷雾串联质谱法(UPLC-ESI-MS/MS),用于定量分析鱼类和脂肪食品中的全氟化合物(PFCs),包括 C6-C14 全氟羧酸(PFCAs)和 C4-C12 全氟磺酸(PFSAs)。UPLC 配备了 PFC 分析试剂盒,以消除背景污染。17 种 PFCs 在 12 分钟内实现了快速基线分离,并且 PFCs 与牛磺脱氧胆酸和 PFCs 的支链异构体的潜在干扰物得到了很好的分离。该方法根据欧盟委员会 2002/657/EC 号委员会法规进行了验证,包括三文鱼、牛肉、鸡蛋和黄油等基质。在 0.02(方法定量下限(MLOQ))、0.2 和 2μg/kg 的浓度水平下,平均加标回收率在 68-117%范围内,相对标准偏差低于 20%。通过内标法评估了基质效应,并发现可以进行校正,特别是对于短链和长链 PFCs。通过与两种认证参考物质的比较验证了准确性。该方法还成功应用于风险评估研究中 200 多种食品样品的分析。

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