title: Liquid-solid sample preparation followed by headspace solid-phase microextraction determination of multiclass pesticides in soil.
abstract: This paper describes development and validation of a multiresidue method for the determination of five pesticides (terbufos, prochloraz, chloridazon, pendimethalin, and fluorochloridone) belonging to different pesticide groups in soil samples by GC/MS, followed by its application in the analysis of some agricultural soil samples. The method is based on a headspace solid-phase microextraction method. Microextraction conditions, namely temperature, extraction time, and NaCI content, were tested and optimized using a 100 microm polydimethylsiloxane fiber. Three extraction solvents [methanol, methanol-acetone (1 + 1, v/v), and methanol-acetone-hexane (2 + 2 + 1, v/v/v)] and the optimum number of extraction steps within the sample preparation stage were optimized for the extraction procedure. LOD values for all the studied compounds were less than 12 microg/kg. Recovery values for multiple analyses of soil samples fortified at 30 microg/kg of each pesticide were higher than 64%. The method was proven to be repeatable, with RSD lower than 15%.
authors.affiliation: Institute of Pesticides and Environmental Protection, Banatska 31b, PO Box 163, 11080 Belgrade, Serbia.
authors.forename: Rada D
authors.initials: RD
authors.lastname: Durović
authors.forename: Tijana M
authors.initials: TM
authors.lastname: Dordević
authors.forename: Ljiljana R
authors.initials: LR
authors.lastname: Santrić
mesh_terms: D002623:Chemistry Techniques, Analytical; D010575:Pesticides / Q000737:chemistry*; D015203:Reproducibility of Results; D012987:Soil / Q000737:chemistry*; D012989:Soil Pollutants / Q000737:chemistry*; D052617:Solid Phase Microextraction / Q000379:methods*
chemical_list: D010575:Pesticides; D012987:Soil; D012989:Soil Pollutants