Determination of 8 Kinds of Super Trace Dechloranes in Soil by Gas Chromatography-Triple Quadrupole Mass Spectrometry with Accelerated Solvent Extraction
  
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KeyWord:accelerated solvent extraction(ASE)  gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS)  soil  dechlorane
  
AuthorInstitution
GUO Xiao-chen,RAO Zhu,LI Xiao-jie,LI Ning,TIAN Qin,PAN Meng,TONG Ling,YANG Zhi-peng,TIAN Fei-fei 1.National Research Center for Geoanalysis;2.Key Laboratory of Ecological Geochemistry,Ministry of Land and Resources,National Research Center;3.China Building Material Test & Certification Group Co.Ltd.;4.Faculty of Materials Science and Chemistry,China University of Geosciences Wuhan;5.Shimadzu Corporation
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Abstract:
      An analytical method of gas chromatography-triple quadrupole mass spectrometry with accelerated solvent extraction(ASE) was established for the determination of 8 kinds of super trace high chlorinated flame retardants dechloranes in surface soil,including mirex,syn declorane,anti declorane,declorane 602,declorane 603,declorane 604,anti Cl10DP and anti Cl11DP.Soil samples were extracted by ASE with hexane-acetone(1∶1,by volume) mixed solvent at 120 ℃,then on line purified with graphitized carbon black and followed by GCB/PSA solid phase extraction column clean up.The extract was analyzed by GC-MS/MS in MRM mode.The spike recoveries of the method for 8 target compounds in soil at low,medium and high levels ranged from 938% to 107%,847% to 101% and 990% to 108% with the relative standard deviations of 51%-13%,52%-83% and 43%-66%,respectively.The detection limits were in the range of 017-110 pg/g.This method was applied in the analysis on the surface soil samples from some urban and rural areas along the Beijing-Hangzhou Grande Canale.Results showed that the detection rates for 4 compounds ie.syn declorane,anti declorane,declorane 602 and mirex were higher than the others,in which the highest rate reached up to 350%,and the highest concentrations of syn declorane,anti declorane in Huaian were 650 ng/g and 244 ng/g,respectively.
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