Pressurised hot water extraction–microporous membrane liquid–liquid extraction coupled on-line with gas chromatography–mass spectrometry in the analysis of pesticides in grapes

Abstract

Pressurised hot water extraction–microporous membrane liquid–liquid extraction was coupled on-line with gas chromatography–mass spectrometry (PHWE–MMLLE–GC–MS) for the analysis of pesticides in grapes. MMLLE serves as a trapping step after PHWE. Water from PHWE is directed to the donor side of the membrane unit and the analytes are extracted to the acceptor solution on the other side. The role of MMLLE is to clean and concentrate the extract before on-line transfer to the GC via a sample loop and an on-column interface using partially concurrent solvent evaporation. The extraction conditions were investigated, and then the quantitative features such as linearity, limit of quantification (LOQ), extraction yield and enrichment factors. LOQs in the range 0.3–1.8 µg kg⁻¹ were achieved. Procymidone and tetradifon were found in the skins of the grapes. The results were in good agreement with those obtained by liquid–solid and ultrasonic extractions.