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加速溶剂萃取-固相萃取净化-超高效液相色谱串联质谱法测定土壤中11种全氟化合物 被引量:29

Analysis of perfluorinated compounds in soil by accelerated solvent extraction combined with ultra performance liquid chromatographytandem mass spectrometry
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摘要 采用超高效液相色谱-串联质谱联用法(UPLC-ESI-MS/MS),建立了分析土壤中11种全氟化合物(PFCs)的方法.以甲醇作为萃取剂,样品经加速溶剂萃取仪(ASE)萃取,固相萃取净化后,使用UPLC-ESI-MS/MS联用仪分析样品中11种PFCs.在6 min内就可快速稳定地将所选取的11种全氟化合物分离,且最低检测浓度为0.518—3.520 pg.g-1之间,这些化合物在土壤中的平均添加回收率在71.2%—119.2%之间.应用此方法测得宜兴市水稻土样品中所选取的PFCs含量为0.006—0.780 ng.g-1之间. A method for the determination of 11 perfluorinated compounds(PFCs) in soil by accelerated solvent extraction(ASE) combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-ESI-MS/MS)was developed.An ACQUITY UPLC BEH C18 column was applied to separate the analytes in 6 min.11 PFCs standards were detected using this method with the limit of detection(LODs) between 0.518—3.520 pg · g-1.Soil samples were extracted by ASE using methanol as solvent.The extracts were concentrated with rotary evaporation and followed by SPE purification before analysis with UPLC-ESI-MS/MS.The recoveries in soil samples were determined to be in the range of 71.2%—119.2% under the spiked conditions.Analysis of real soil samples collected in Yixing showed that all of the 11 PFCs were detected at the level of 0.006—0.780 ng · g-1.Overall,the data showed that the method developed in this study is sensitive,accurate and suitable for analyzing trace PFCs in soil.
出处 《环境化学》 CAS CSCD 北大核心 2012年第1期113-119,共7页 Environmental Chemistry
基金 环保公益性行业科研专项(200909089)中央级公益性科研院所基本科研业务专项
关键词 超高效液相色谱串联质谱法 快速溶剂萃取 全氟化合物 土壤 固相萃取 ultra performance liquid chromatography tandem mass spectrometry ASE perfluorinated compounds soil SPE.
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