Application of liquid-phase microextraction and on-column derivatization combined with gas chromatography–mass spectrometry to the determination of carbamate pesticides

A method has been established for the determination of five carbamate pesticides in water samples using liquid-phase microextraction (LPME) followed by on-column derivatization and gas chromatography–mass spectrometric (GC–MS) determination. Trimethylphenylammonium hydroxide (TMPAH) and trimethylsulfonium hydroxide (TMSH) were used as derivatization reagent for extracts prior to GC–MS analysis as carbamate pesticides are thermally labile compounds. Parameters that affect the extraction efficiency (selection of organic solvent and extraction time) and derivatization efficiency (choice of derivatization reagent and concentration of derivatization reagent) were investigated. The proposed method provided good enrichment factors up to 224, with reproducibility ranging from 4.86 to 7.81%, and good linearity from 1 to 400 μg/L. The limits of detection (LODs) ranged between 0.2 and 0.8 μg/L (S/N = 3) using GC–MS with selective ion monitoring. This method was applied to the determination of carbamate pesticides in tap water and waste water.