Coupling ASE, sylilation and SPME-GC/MS for the analysis of current-used pesticides in atmosphere

Caroline Raeppel, Marie Fabritius, Marie Nief, Brice M.R. Appenzeller, Maurice Millet*

*Corresponding author for this work

Research output: Contribution to journalArticleResearchpeer-review

38 Citations (Scopus)


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 m3 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.

Original languageEnglish
Pages (from-to)24-29
Number of pages6
Publication statusPublished - Apr 2014


  • GC/MS
  • Low-volume sampling
  • Non-agricultural pesticides
  • Solid phase micro-extraction
  • Sylilation


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