Solid-phase microextraction method for the determination of atrazine and four organophosphorus pesticides in soil samples by gas chromatography

J Chromatogr A. 2001 Dec 21;939(1-2):13-21. doi: 10.1016/s0021-9673(01)01332-2.

Abstract

A simple and rapid solid-phase microextraction (SPME) based method is presented for the simultaneous determination of atrazine and four organophosphorus (i.e. parathion-methyl, chlorpyriphos, methidathion and carbophenothion) in soils. After optimisation of the different experimental variables affecting the SPME of the target compounds from aqueous solutions by using an experimental design, a consensus strategy was adopted which allowed the use of the SPME method developed for the simultaneous screening of all the analytes selected. The complete analytical procedure finally proposed consisted of a 15-min ultrasonic extraction of the target compounds from a 0.5-g soil sample with 5 ml of methanol and the dilution of this extract to up 10% methanol followed by the addition of NaCl to a final concentration of 10% (w/v). The analytes in this aqueous extract were preconcentrated for 30 min in the SPME fiber and subsequently desorbed by heating of the fiber at 260 degrees C for 5 min in the gas chromatograph injection port. Final determination was carried out with an electron-capture detector. The recoveries of the pesticides studied in soils ranged from 72 to 123%, except for atrazine, and the SDs were below 16%. The feasibility of the procedure finally proposed for the screening of the endogenous pesticides irrespective of the properties of the soil selected has been shown.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Atrazine / analysis*
  • Chromatography, Gas / methods*
  • Herbicides / analysis*
  • Insecticides / analysis*
  • Organophosphorus Compounds*
  • Sensitivity and Specificity
  • Soil Pollutants / analysis*

Substances

  • Herbicides
  • Insecticides
  • Organophosphorus Compounds
  • Soil Pollutants
  • Atrazine