title: Fast low-pressure gas chromatography-mass spectrometry method for the determination of multiple pesticides in grapes, musts and wines.
abstract: A fast method using low-pressure gas chromatography coupled to mass spectrometry (LP-GC/MS) was implemented and optimized to yield a complete separation of 27 representative pesticides in grapes, musts and wines. Extraction was performed with acetonitrile, applying quick, easy, cheap, effective, rugged and safe (QuEChERS) methodology. Several LP-GC/MS conditions such as column temperature, injection conditions, flow rate, MS conditions and matrix effects were evaluated to achieve the fastest separation with the highest sensitivity in MS detection (selected ion monitoring mode). After optimization, all 27 pesticides were extracted, chromatographically separated and detected in less than 20 min. Acceptable recoveries for nearly all pesticides at three different spiking levels (from 0.04 to 2.5 microg/g) were achieved with good repeatability (from 3 to 21%). Limits of quantification (from 0.02 to 5 microg/g) were lower than the maximum limit of residues, when established for pesticides.
authors.affiliation: REQUIMTE, Serviço de Bromatologia, Faculty of Pharmacy, University of Porto, Rua Aníbal Cunha 164, 4099-030 Porto, Portugal. sara.cunha@ff.up.pt
authors.forename: S C
authors.initials: SC
authors.lastname: Cunha
authors.forename: J O
authors.initials: JO
authors.lastname: Fernandes
authors.forename: A
authors.initials: A
authors.lastname: Alves
authors.forename: M B P P
authors.initials: MB
authors.lastname: Oliveira
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D010575:Pesticides / Q000032:analysis*; D011312:Pressure; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012997:Solvents / Q000737:chemistry; D013997:Time Factors; D027843:Vitis / Q000737:chemistry*; D014920:Wine / Q000032:analysis*
chemical_list: D000097:Acetonitriles; D010575:Pesticides; D012997:Solvents; C032159:acetonitrile