title: Coupling ASE, sylilation and SPME-GC/MS for the analysis of current-used pesticides in atmosphere.
abstract: An analytical methodology using Accelerated Solvent Extraction (ASE) and a sylilation procedure coupled to Solid Phase Micro-Extraction (SPME) and GC/MS was developed for the determination of 31 pesticides of different chemical classes (urea, phenoxy acids, pyrethrenoïds, etc.) commonly used in non-agricultural areas in atmospheric samples. This methodology was developed to evaluate the outdoor atmospheric contamination by non-agricultural pesticides. Pesticides were simultaneously sampled on glass fibre filters and on XAD-2 resin traps by using a low volume sampler (Partisol) for 1 week. Traps were extracted by Accelerated Solvent Extraction (ASE) with acetonitrile and concentrated to 1 mL by using a rotary evaporator. 500 µL of the extract was dissolved in 19.5 mL of 1.5% NaCl acidified water (pH=3) and SPME extracted by PA fibre for 55 min at 50 °C. Since most of the studied pesticides are polar or thermo-labile, a derivatisation step by injection of 2 µL of MtBSTFA just before SPME desorption was done. MtBSTFA was chosen since it delivers very specific ions on electronic impact (m/z=M-57). Detection limits varied between 5 and 179 ng resin(-1) and between 0.3 and 126 ng filter(-1) corresponding to 2 and 750 pg m(-3) and 30 and 1165 pg m(-3) for 168 m(3) of air pumped through traps. Quantification limits varied between 18 and 595 ng resin(-1) and between 1 and 420 ng filter(-1) corresponding to 107 and 3542 pg m(-3) and 6 and 2500 pg m(-3) for 168 m(3) of air pumped through traps. Uncertainties varied between 7.2% and 39.6% and between 7.2% and 53.4% respectively for filter and resin. The method was used for the analysis of atmospheric samples collected in a background urban site of Strasbourg (east of France) during spring and summer 2010.
authors.affiliation: Groupe de Physico-Chimie de l'Atmosphère - ICPEES (UMR 7515 CNRS, Université de Strasbourg), 1, rue Blessig, 67084 Strasbourg Cedex, France; Laboratory of Analytical Human Biomonitoring, CRP-Santé, Université du Luxembourg, 162A Avenue de la Faïencerie, L-1511, Luxembourg.
authors.forename: Caroline
authors.initials: C
authors.lastname: Raeppel
authors.affiliation: Groupe de Physico-Chimie de l'Atmosphère - ICPEES (UMR 7515 CNRS, Université de Strasbourg), 1, rue Blessig, 67084 Strasbourg Cedex, France.
authors.forename: Marie
authors.initials: M
authors.lastname: Fabritius
authors.affiliation: Groupe de Physico-Chimie de l'Atmosphère - ICPEES (UMR 7515 CNRS, Université de Strasbourg), 1, rue Blessig, 67084 Strasbourg Cedex, France.
authors.forename: Marie
authors.initials: M
authors.lastname: Nief
authors.affiliation: Laboratory of Analytical Human Biomonitoring, CRP-Santé, Université du Luxembourg, 162A Avenue de la Faïencerie, L-1511, Luxembourg.
authors.forename: Brice M R
authors.initials: BM
authors.lastname: Appenzeller
authors.affiliation: Groupe de Physico-Chimie de l'Atmosphère - ICPEES (UMR 7515 CNRS, Université de Strasbourg), 1, rue Blessig, 67084 Strasbourg Cedex, France. Electronic address: mmillet@unistra.fr.
authors.forename: Maurice
authors.initials: M
authors.lastname: Millet
mesh_terms: D000393:Air Pollutants / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D057230:Limit of Detection; D010575:Pesticides / Q000032:analysis*; D052617:Solid Phase Microextraction
chemical_list: D000393:Air Pollutants; D010575:Pesticides
keywords: GC/MS; Low-volume sampling; Non-agricultural pesticides; Solid phase micro-extraction; Sylilation