On-line solid-phase extraction–liquid chromatography–particle beam mass spectrometry and gas chromatography–mass spectrometry of carbamate pesticides

Abstract
On-line solid-phase extraction–liquid chromatography–particle beam mass spectrometry (SPE–LC–PB-MS) was used to study 32 carbamates and 11 of their transformation products in environmental water samples. The analytes were enriched from 100 ml samples on Bondesil-C18/OH, packed in a 10 mm × 3.0 mm id precolumn, eluted on-line with a gradient of methanol–0.1 mol l–1 ammonium acetate to a C18 analytical column and detected by PB-MS. Detection limits of 12 carbamates and five degradation products were 0.1–8 µg l–1 in surface water, using full-scan electron impact mode detection. The RSDs of the retention times were 0.05–0.2% and those of peak areas 5–35%. Twenty-eight analytes proved to be amenable to GC with detection limits of 0.05–3 ng injected on-column. When using the same mass spectrometer, the spectra obtained by LC–PB-MS and GC–MS were identical.

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