Chinese Journal of Chromatography

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Determination of trace organochlorine pesticides in soil using isotope dilution-high resolution gas chromatography-high resolution mass spectrometry

HUANG Wenjun1,2, GAO Lirong1*, GONG Aijun2, LI Cheng1, WANG Pu1, FU Shan1, XIAO Ke1, ZHANG Bing1, LIU Wenbin1   

  1. 1. Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China; 2. Department of Chemistry, School of Applied Science, University of Science and Technology Beijing, Beijing 100083, China
  • Received:2010-01-14 Revised:2010-02-14 Online:2010-05-28 Published:1980-09-25
  • Contact: GAO Lirong

Abstract: A method for the determination of trace organochlorine pesticides (OCPs) in soil using isotope dilution and high resolution gas chromatography-high resolution mass spectrometry (ID-HRGC-HRMS) was developed. The sample was extracted by accelerated solvent extractor (ASE) and cleaned-up by a Florisil solid phase extraction (SPE) cartridge. The analytes were separated by HRGC on a DB-5MS column (30 m×0.25 mm×0.25 μm) and determined by HRMS. The identifications of OCPs were based on the retention time of 13C-labelled standard and the abundance ratio of the two exact mass-to-charge ratios. The quantitative analysis was performed using the ratios of the integrated areas of the 13C-labelled standards. This method has the recoveries ranging from 77.3% to 114.5% and the relative standard deviations (RSD) less than 10.81% (n=5). The limits of detection (LODs) of this method for all OCPs were lower than 0.04 pg/g. The results indicated that the method is rapid, selective and sensitive for precise determination requirements of organochlorine pesticides at trace level in soil.

Key words: isotope dilution, organochlorine pesticide, soil , high resolution gas chromatography-high resolution mass spectrometry (HRGC-HRMS)