title: Target analysis and retrospective screening of veterinary drugs, ergot alkaloids, plant toxins and other undesirable substances in feed using liquid chromatography-high resolution mass spectrometry.
abstract: A comprehensive strategy combining a quantitative method for 77 banned veterinary drugs, mycotoxins, ergot alkaloids and plant toxins, and a post-target screening for 425 substances including pesticides and environmental contaminants in feed were developed using a QuEChERS-based extraction and an ultra-high performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-HRMS). The quantitative method was validated after previous statistical optimisation of the main parameters governing ionisation, and presented recoveries ranging, in general, from 80 to 120%, with a precision in terms of Relative Standard Deviation (RSD) lower than 20%. The full-scan accurate mass data were acquired with a resolving power of 50000 FWHM and a mass accuracy lower than 5ppm. The method LOQ was lower than 12.5µgkg(-1) for the majority of the veterinary drugs and plant toxins and 20µgkg(-1) for ergot alkaloids. For post-target screening a customised theoretical database including the exact mass, the polarity of acquisition and the expected adducts was built and used for post-run retrospective screening. The analytical strategy was applied to 32 feed samples collected from farms of the Valencia Region (Spain). Florfenicol, zearalenone and atropine were identified and quantified at concentrations around 10µgkg(-1). In the post-target screening of the real samples, Sulfadiazine, Thrimetoprin and Pirimiphosmethyl were tentatively identified.
authors.affiliation: Public Health Laboratory of Valencia, Avenida Catalunya 21, 46020 Valencia, Spain; Foundation for the Promotion of Health and Biomedical Research in the Valencian Region, FISABIO - Public Health, Avenida Catalunya 21, 46020 Valencia, Spain.
authors.forename: Nuria
authors.initials: N
authors.lastname: León
authors.affiliation: Analytical Chemistry Department, Universidad de Valencia, Edifici Jeroni Muñoz, 50, Dr. Moliner, Burjassot, 46100 Valencia, Spain.
authors.forename: Agustín
authors.initials: A
authors.lastname: Pastor
authors.affiliation: Public Health Laboratory of Valencia, Avenida Catalunya 21, 46020 Valencia, Spain; Foundation for the Promotion of Health and Biomedical Research in the Valencian Region, FISABIO - Public Health, Avenida Catalunya 21, 46020 Valencia, Spain; Analytical Chemistry Department, Universidad de Valencia, Edifici Jeroni Muñoz, 50, Dr. Moliner, Burjassot, 46100 Valencia, Spain. Electronic address: yusa_vic@gva.es.
authors.forename: Vicent
authors.initials: V
authors.lastname: Yusà
mesh_terms: D000470:Alkaloids / Q000032:analysis; D000821:Animal Feed / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid; D004785:Environmental Pollutants / Q000032:analysis*; D005506:Food Contamination / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods; D010575:Pesticides / Q000032:analysis; D015203:Reproducibility of Results; D014118:Toxins, Biological / Q000032:analysis; D019155:Veterinary Drugs / Q000032:analysis
chemical_list: D000470:Alkaloids; D004785:Environmental Pollutants; D010575:Pesticides; D014118:Toxins, Biological; D019155:Veterinary Drugs
keywords: Animal feed; Ergot alkaloids; LC–HRMS; Orbitrap; Retrospective analysis; Veterinary drugs