title: Determination of spiroxamine residues in grapes, must, and wine by gas chromatography/ion trap-mass spectrometry.
abstract: Analytical methodology was developed and validated for the determination of spiroxamine residues in grapes, must, and wine by gas chromatography/ion trap-mass spectrometry (GC/IT-MS). Two extraction procedures were used: the first involved grapes, must, and wine extraction with alkaline cyclohexane-dichloromethane (9 + 1, v/v) solution, and the second grape extraction with acetone, dichloromethane, and petroleum ether. In both procedures, the extract was centrifuged, evaporated to dryness, and reconstituted in cyclohexane or 2,2,4-trimethylpentane-toluene (9 + 1, v/v), respectively. Spiroxamine diastereomers A and B were determined by GC/IT-MS, and a matrix effect was observed in the case of grapes but not in must and wine. Recovery of spiroxamine from fortified samples at 0.02 to 5.0 mg/kg ranged from 78-102% for grapes and must, with relative standard deviation (RSD) <13%; for red and white wines, recoveries ranged from 90 to 101% with RSD <9%. The limit of quantification was 0.02 mg/kg for grapes, must, and wine or 0.10 mg/kg for grapes, depending on the extraction procedure used.
authors.affiliation: University of Thessaly, Department of Agriculture, Analytical Chemistry and Pesticides Laboratory, Crop Production and Rural Environment, Fytokou Str, 384 46, Nea Ionia - Volos, Greece. ntsirop@uth.gr
authors.forename: Nicholas G
authors.initials: NG
authors.lastname: Tsiropoulos
authors.forename: Konstantinos
authors.initials: K
authors.lastname: Liapis
authors.forename: Dimitrios T
authors.initials: DT
authors.lastname: Likas
authors.forename: George E
authors.initials: GE
authors.lastname: Miliadis
mesh_terms: D000096:Acetone / Q000032:analysis; D000473:Alkanes / Q000032:analysis; D000588:Amines / Q000032:analysis*; D002623:Chemistry Techniques, Analytical / Q000379:methods*; D002845:Chromatography; D002849:Chromatography, Gas / Q000379:methods*; D003510:Cyclohexanes / Q000032:analysis; D004350:Drug Residues; D005504:Food Analysis; D005506:Food Contamination; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006863:Hydrogen-Ion Concentration; D007477:Ions; D013058:Mass Spectrometry / Q000379:methods; D008752:Methylene Chloride / Q000032:analysis; D008956:Models, Chemical; D009795:Octanes / Q000032:analysis; D010573:Pesticide Residues / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013141:Spiro Compounds / Q000032:analysis* / Q000737:chemistry; D013997:Time Factors; D014050:Toluene / Q000032:analysis; D027843:Vitis / Q000378:metabolism*; D014920:Wine
chemical_list: D000473:Alkanes; D000588:Amines; D003510:Cyclohexanes; D007477:Ions; D009795:Octanes; D010573:Pesticide Residues; D013141:Spiro Compounds; D000096:Acetone; D014050:Toluene; D008752:Methylene Chloride; C004544:naphtha; C510887:spiroxamine; C045798:2,2,4-trimethylpentane