Analysis of hydroxylated polybrominated diphenyl ethers in plant samples using ultra performance liquid chromatography-mass spectrometry

作     者：WANG Sen WU Tong HUANG HongLin PING Hua LU AnXiang ZHANG ShuZhen 

作者机构：State Key Laboratory of Environmental Chemistry and Ecotoxicology Research Center for Eco-Environmental Sciences Chinese Academy of Sciences Beijing 100085 China Beijing Research Center for Agri-food Testing and Farmland Monitoring Beijing 100097 China 

出 版 物：《Science China Chemistry》 (中国科学（化学英文版）)

年 卷 期：2011年第54卷第11期

页      面：1782-1788页

核心收录：

学科分类：0710[理学-生物学] 071001[理学-植物学] 081704[工学-应用化学] 07[理学] 08[工学] 0817[工学-化学工程与技术] 070302[理学-分析化学] 0703[理学-化学] 

基　　金：funded by the National Natural Science Foundation of China (40730740 & 20921063) the National Basic Research Program of China (2009CB421603) 

主　　题：OH-PBDE plant extraction ultra performance liquid chromatography mass spectrometry 

摘      要：A method was developed for the analysis of hydroxylated brominated diphenyl ethers (OH-PBDEs) in plant samples using an ultra performance liquid chromatography-triple quadrupole mass spectrometer (UPLC-ESI-MS/MS) in negative mode. Plant samples were extracted and cleaned up through florisil column, resolved on a 100 mm C18 column with linear gradient elution and detected by mass spectrometry in multiple reaction monitoring (MRM) mode. The method provided good recoveries rang- ing from 68.2% to 94.6%, relative standard deviation (RSD) in the range of 3.2% - 9.1%, and limits of quantification (LOQ) defined as the signal-to-noise ratio of 10 of 0.3-2.1 ng/g. It allowed a fast separation and sensitive quantification of the isomers and homologues of seven OH-PBDE congeners 2′-OH-BDE-3, 3′-OH-BDE-7, 4′-OH-BDE-17, 3′-OH-BDE-28, 3-OH-BDE-47, 5-OH-BDE-47 and 6-OH-BDE-47. The method was successfully applied to identify and quantify the formation of hydroxylat- ed metabolites in alfalfa exposed to BDE-209. Five OH-PBDEs were detected in plant tissues, and more congeners were found in roots than in shoots. To our knowledge, this work represents the first attempt to validate UPLC-MS/MS method to quantify OH-PBDEs in plant samples without derivatization.