title: 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.
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.
authors.affiliation: Laboratory of Process, Environment and Energy Engineering (LEPAE), Chemical Engineering Department, Engineering Faculty, University of Porto, Rua Dr. Roberto Frias, 4200-465, Porto, Portugal. pribeiro@fe.up.pt
authors.forename: Paulo
authors.initials: P
authors.lastname: Herbert
authors.forename: Simone
authors.initials: S
authors.lastname: Morais
authors.forename: Paula
authors.initials: P
authors.lastname: Paíga
authors.forename: Arminda
authors.initials: A
authors.lastname: Alves
authors.forename: Lúcia
authors.initials: L
authors.lastname: Santos
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006843:Hydrocarbons, Chlorinated / Q000032:analysis* / Q000528:radiation effects; D008872:Microwaves; D010575:Pesticides / Q000032:analysis* / Q000528:radiation effects; D012680:Sensitivity and Specificity; D012987:Soil / Q000032:analysis*; D052617:Solid Phase Microextraction / Q000379:methods*; D013696:Temperature
chemical_list: D006843:Hydrocarbons, Chlorinated; D010575:Pesticides; D012987:Soil