Analysis of Organochlorine Pesticides in Soil by GC-MS with Solid Phase Extraction and Their Matrix Effects Study
  
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KeyWord:soil  organochlorine  clean-up  injection condition  matrix effect
  
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LIU Ling-ling,MENG Tian-tian,DONG Xi-liang,REN Wei,ZHANG Li-jun Jinan Environmental Research Institute
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Abstract:
      A method of solid phase extraction/gas chromatography-mass spectrometry was developed for the simultaneous determination of 23 organochlorine pesticides in soil.And different matrix effect compensation approaches were studied.Soil samples were extracted with n hexane-acetone(1∶1,by volume),then purified with a florisil column,and finally detected by GC-MS.Medium or strong matrix effects existed in 7 organic chlorines,which was controlled within 20% for all the 23 organochlorines when 10 mL dichloromethane∶n-hexane(1∶9,by volume) and 10 mL acetone∶n hexane(1∶9,by volume) were selected as the eluents of solid phase extraction,and the pulse pressure was set at 275.8 kPa.Results showed that there was a good linear relationship of the method in the concentration range of 04-10 μg·mL-1 with correlation coefficients(r2) no less than 0.999 2.The limits of detection and limits of quantitation were in the ranges of 1.0-8.6 μg·kg-1 and 4.0-34.4 μg·kg-1,respectively.The average recoveries for blank soil at spiked levels of 20,60 and 100 μg·kg-1 ranged from 46.3% to 109%,with relative standard deviations(RSDs,n=6) of 0.68%-15%.Five organochlorine pesticides,including α-BHC,γ-BHC,p,p′-DDE,endrin aldehyde,p,p′-DDT were detected in a soil sample.
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