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凝胶渗透色谱-分散固相萃取-液相色谱串联质谱法同时测定食用油中的全氟化合物。

Simultaneous Determination of Perfluorinated Compounds in Edible Oil by Gel-Permeation Chromatography Combined with Dispersive Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry.

机构信息

Key Laboratory of Agro-product Quality and Safety, Institute of Quality Standards & Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences , Beijing 100081, China.

出版信息

J Agric Food Chem. 2015 Sep 30;63(38):8364-71. doi: 10.1021/acs.jafc.5b03903. Epub 2015 Sep 22.

Abstract

A simple analytical method was developed for the simultaneous analysis of 18 perfluorinated compounds (PFCs) in edible oil. The target compounds were extracted by acetonitrile, purified by gel permeation chromatography (GPC) and dispersive solid-phase extraction (DSPE) using graphitized carbon black (GCB) and octadecyl (C18), and analyzed by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ES-MS/MS) in negative ion mode. Recovery studies were performed at three fortification levels. The average recoveries of all target PFCs ranged from 60 to 129%, with an acceptable relative standard deviation (RSD) (1-20%, n = 3). The method detection limits (MDLs) ranged from 0.004 to 0.4 μg/kg, which was significantly improved compared with the existing liquid-liquid extraction and cleanup method. The method was successfully applied for the analysis of all target PFCs in edible oil samples collected from markets in Beijing, China, and the results revealed that C6-C10 perfluorocarboxylic acid (PFCAs) and C7 perfluorosulfonic acid PFSAs were the major PFCs detected in oil samples.

摘要

建立了一种同时分析食用油中 18 种全氟化合物(PFCs)的简单分析方法。采用乙腈提取目标化合物,经凝胶渗透色谱(GPC)和石墨化碳黑(GCB)和十八烷基(C18)分散固相萃取(DSPE)净化,采用液相色谱-电喷雾串联质谱(LC-ES-MS/MS)在负离子模式下进行分析。在三个加标水平进行了回收率研究。所有目标 PFC 的平均回收率在 60-129%之间,相对标准偏差(RSD)(1-20%,n=3)可接受。方法检测限(MDLs)范围为 0.004-0.4μg/kg,与现有的液液萃取和净化方法相比有显著提高。该方法成功应用于分析中国北京市场采集的食用油样品中的所有目标 PFCs,结果表明,C6-C10 全氟羧酸(PFCAs)和 C7 全氟磺酸(PFSAs)是油样中主要检测到的 PFCs。

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