PMID- 19073064 OWN - NLM STAT- PubMed-not-MEDLINE DCOM- 20121002 LR - 20081216 IS - 1873-3573 (Electronic) IS - 0039-9140 (Linking) VI - 73 IP - 3 DP - 2007 Sep 30 TI - Determination of phosmet and its metabolites in olives by matrix solid-phase dispersion and gas chromatography-mass spectrometry. PG - 514-22 LID - 10.1016/j.talanta.2007.04.014 [doi] AB - An accurate method based on matrix solid-phase dispersion (MSPD), and gas chromatography-mass spectrometry (GC/MS) was developed for determination of phosmet residues and its metabolites (phosmet-oxon, phthalimide, N-hydroxymethylphthalimide, and phthalic acid) in olive fruits. After testing different sorbents and eluents for MSPD extraction, C(18) and acetonitrile were found to be the most appropriate for clean-up of the samples, in terms of yields and efficient removal of interfering compounds. All analytes were determined in selective ion monitoring (SIM) mode following a derivatization step with N,O-bis-trimethylsilyltrifluoroacetamide (BSTFA) containing 1% of trimethylchlorosilane (TMCS), except for phosmet and phosmet-oxon which were analyzed directly. The method showed suitable linearity (correlation coefficients higher than 0.8919 for all the compounds) and suitable sensitivity (limit of detection lower than 0.06mg/kg). It was successfully applied in the analysis of olive fruits collected during the preharvest interval and olive oil. Phosmet residues found in all samples were lower than the maximum residue limits established by legislation (2mg/kg). FAU - Cunha, Sara C AU - Cunha SC AD - REQUIMTE/Servico de Bromatologia, Faculdade de Farmacia, Universidade do Porto, Rua Anibal Cunha 164, 4099-030 Porto, Portugal. FAU - Fernandes, Jose O AU - Fernandes JO FAU - Beatriz, M AU - Beatriz M FAU - Oliveira, P P AU - Oliveira PP LA - eng PT - Journal Article DEP - 20070424 PL - Netherlands TA - Talanta JT - Talanta JID - 2984816R EDAT- 2007/09/30 00:00 MHDA- 2007/09/30 00:01 CRDT- 2008/12/17 09:00 PHST- 2007/01/17 00:00 [received] PHST- 2007/03/28 00:00 [revised] PHST- 2007/04/11 00:00 [accepted] PHST- 2008/12/17 09:00 [entrez] PHST- 2007/09/30 00:00 [pubmed] PHST- 2007/09/30 00:01 [medline] AID - S0039-9140(07)00304-9 [pii] AID - 10.1016/j.talanta.2007.04.014 [doi] PST - ppublish SO - Talanta. 2007 Sep 30;73(3):514-22. doi: 10.1016/j.talanta.2007.04.014. Epub 2007 Apr 24.