title: Liquid chromatography quadrupole time-of-flight mass spectrometry analysis of carbosulfan, carbofuran, 3-hydroxycarbofuran, and other metabolites in food.
abstract: The potential of liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QqTOF-MS) to identify and confirm carbosulfan and seven of its main metabolites (carbofuran, 3-hydroxycarbofuran, 3-ketocarbofuran, 3-hydroxy-7-phenol carbofuran, 3-keto-7-phenolcarbofuran, 7-phenolcarbofuran, dibutylamine) at trace levels from food is explored for the first time. The analytical method developed consists of pressurized liquid extraction (PLE) and LC-QqTOF-MS in positive ion mode, which attains unequivocal identification and quantification of the studied compounds in food, at levels well below of those of concern (0.05 mg/kg for the sum of carbosulfan, carbofuran, and 3-hydroxycarbofuran). PLE recoveries ranged from 55 to 94% with limits of quantification from 10 (for carbosulfan, carbofuran, 3-hydroxycarbofuran, and dibutylamine) to 70 microg/kg (3-keto-7-phenolcarbofuran). The method is precise, with relative standard deviations varying between 5 and 11% for the repeatability (within-day) and 8-13% for the reproducibility (interday). This method was used to monitor the presence and fate of the target compounds in orange, potato, and rice crops treated with a commercial product containing carbosulfan. Field degradation studies show that carbofuran, 3-hydroxycarbofuran, and dibutylamine are the main degradation products formed in the environmental disappearance of carbosulfan.
authors.affiliation: Laboratori de Bromatologia i Toxicologia, Facultat de Farmàcia, Universitat de València, Avenue Vicent Andrés Estellés s/n, 46100 Burjassot, Spain. carla.soler@uv.es
authors.forename: Carla
authors.initials: C
authors.lastname: Soler
authors.forename: Brett
authors.initials: B
authors.lastname: Hamilton
authors.forename: Ambrose
authors.initials: A
authors.lastname: Furey
authors.forename: Kevin J
authors.initials: KJ
authors.lastname: James
authors.forename: Jordi
authors.initials: J
authors.lastname: Mañes
authors.forename: Yolanda
authors.initials: Y
authors.lastname: Picó
mesh_terms: D002082:Butylamines / Q000032:analysis*; D002219:Carbamates / Q000032:analysis*; D002235:Carbofuran / Q000031:analogs & derivatives* / Q000032:analysis* / Q000737:chemistry; D002853:Chromatography, Liquid / Q000379:methods; D005504:Food Analysis; D015394:Molecular Structure; D012680:Sensitivity and Specificity; D019032:Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization / Q000379:methods*
chemical_list: C518702:3-hydroxy-7-phenol carbofuran; C518700:3-keto-7-phenolcarbofuran; C518701:7-phenolcarbofuran; D002082:Butylamines; D002219:Carbamates; C032069:3-ketocarbofuran; C045274:dibutylamine; C028403:3-hydroxycarbofuran; D002235:Carbofuran; C035038:carbosulfan