Development and validation of a novel method for the analysis of chlorinated pesticides in soils using microwave-assisted extraction-headspace solid phase microextraction and gas chromatography-tandem mass spectrometry

Anal Bioanal Chem. 2006 Feb;384(3):810-6. doi: 10.1007/s00216-005-0211-6. Epub 2005 Dec 22.

Abstract

A new procedure for determining eleven organochlorine pesticides in soils using microwave-assisted extraction (MAE) and headspace solid phase microextraction (HS-SPME) is described. The studied pesticides consisted of mirex, alpha- and gamma-chlordane, p,p'-DDT, heptachlor, heptachlor epoxide isomer A, gamma-hexachlorocyclohexane, dieldrin, endrin, aldrine and hexachlorobenzene. The HS-SPME was optimized for the most important parameters such as extraction time, sample volume and temperature. The present analytical procedure requires a reduced volume of organic solvents and avoids the need for extract clean-up steps. For optimized conditions the limits of detection for the method ranged from 0.02 to 3.6 ng/g, intermediate precision ranged from 14 to 36% (as CV%), and the recovery from 8 up to 51%. The proposed methodology can be used in the rapid screening of soil for the presence of the selected pesticides, and was applied to landfill soil samples.

Publication types

  • Research Support, Non-U.S. Gov't
  • Validation Study

MeSH terms

  • Gas Chromatography-Mass Spectrometry / methods*
  • Hydrocarbons, Chlorinated / analysis*
  • Hydrocarbons, Chlorinated / radiation effects
  • Microwaves
  • Pesticides / analysis*
  • Pesticides / radiation effects
  • Sensitivity and Specificity
  • Soil / analysis*
  • Solid Phase Microextraction / methods*
  • Temperature

Substances

  • Hydrocarbons, Chlorinated
  • Pesticides
  • Soil