Simultaneous determination of traces of pyrethroids, organochlorines and other main plant protection agents in agricultural soils by headspace solid-phase microextraction-gas chromatography

J Chromatogr A. 2008 Apr 25;1188(2):154-63. doi: 10.1016/j.chroma.2008.02.080. Epub 2008 Mar 2.

Abstract

A solvent-free and simple method based on headspace solid-phase microextraction (HS-SPME) was developed in order to determine simultaneously 36 common pesticides and breakdown products (mostly pyrethroids and organochlorine compounds) in soil. The analysis was carried out by gas chromatography with micro-electron-capture detection (GC-microECD). As far as we know, this is the first study about the SPME of pyrethroid insecticides from soil. Factors such as extraction temperature, matrix modification by addition of water, salt addition (% NaCl) and fiber coating were considered in the optimization of the HS-SPME. To this end, a 3 x 2(3-1) fractional factorial design was performed. The results showed that temperature and fiber coating were the most significant variables affecting extraction efficiency. A suitable sensitivity for all investigated compounds was achieved at 100 degrees C by extracting soil samples wetted with 0.5 mL of ultrapure water (0% NaCl) employing a polyacrylate (PA) coating fiber. Using the recommended extraction conditions with GC-microECD, a linear calibration could be achieved over a range of two orders of magnitude for both groups of analytes. Limits of detection (LODS) at the sub-ng g(-1) level were attained and relative standard deviations (RSDs) were found to be lower than 14% for both groups of pesticides. Matrix effects were investigated by the analysis of different soil samples fortified with the target compounds. The method accuracy was assessed and good recovery values (>70%, in most cases) were obtained. The method was also validated with a certified reference material (RTC-CRM818-050), which was quantified using a standard addition protocol. Finally, the proposed HS-SPME-GC-microECD methodology was further applied to the screening of environmental soil samples for the presence of the target pesticides.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Agriculture*
  • Chromatography, Gas
  • Hydrocarbons, Chlorinated / analysis*
  • Pesticides / analysis*
  • Pesticides / isolation & purification
  • Pyrethrins / analysis*
  • Reference Standards
  • Reproducibility of Results
  • Soil / analysis*
  • Solid Phase Microextraction / methods*
  • Solvents
  • Temperature

Substances

  • Hydrocarbons, Chlorinated
  • Pesticides
  • Pyrethrins
  • Soil
  • Solvents