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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
引用本文:王懿,孔德洋,单正军,谭丽超.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[J].环境化学,2012,31(1):113-119.
作者姓名:王懿  孔德洋  单正军  谭丽超
作者单位:1. 南京农业大学资源与环境科学学院,南京,210095/环境保护部南京环境科学研究所,南京,210042
2. 环境保护部南京环境科学研究所,南京,210042
基金项目:环保公益性行业科研专项,中央级公益性科研院所基本科研业务专项
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.

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

Analysis of perfluorinated compounds in soil by accelerated solvent extraction combined with ultra performance liquid chromatographytandem mass spectrometry
WANG Yi,KONG Deyang,SHAN Zhengjun,TAN Lichao.Analysis of perfluorinated compounds in soil by accelerated solvent extraction combined with ultra performance liquid chromatographytandem mass spectrometry[J].Environmental Chemistry,2012,31(1):113-119.
Authors:WANG Yi  KONG Deyang  SHAN Zhengjun  TAN Lichao
Institution:1,2(1.College of Resources and Environmental Sciences,Nanjing Agricultural University,Nanjing,210095,China; 2.Nanjing Institute of Environmental Science,Ministry of Environmental Protection of the People′s Republic of China,Nanjing,210042,China)
Abstract: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.
Keywords:ultra performance liquid chromatography tandem mass spectrometry  ASE  perfluorinated compounds  soil  SPE
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