title: Analysis of 76 veterinary pharmaceuticals from 13 classes including aminoglycosides in bovine muscle by hydrophilic interaction liquid chromatography-tandem mass spectrometry.
abstract: A multiresidue/multiclass method for the simultaneous determination of 76 veterinary drugs and pharmaceuticals in bovine muscle tissue has been developed and validated according to the requirements of European Commission Decision 2002/657/EC. The analytes belong in 13 different classes, including aminoglycoside antibiotics, whose different physicochemical properties (extremely polar character) render their simultaneous determination with other veterinary drugs quite problematic. The method combines a two-step extraction procedure (extraction with acetonitrile followed by an acidic aqueous buffer extraction) with hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) determination, allowing confirmation and quantification in a single chromatographic run. Further cleanup with solid phase extraction was performed using polymeric SPE cartridges. A thorough ionization study of aminoglycosides was performed in order to increase their sensitivity and significant differences in the abundance of the precursor ions of the analytes were revealed, depending on the composition of the mobile phase tested. Further gradient elution optimization and injection solvent optimization were performed for all target analytes.The method was validated according to the European Commission Decision 2002/657. Quantitative analysis was performed by means of standard addition calibration. Recoveries varied from 37.4% (bromhexine) to 106% (kanamycin) in the lowest validation level and 82% of the compounds showed recovery >70%. Detection capability (CCβ) varied from 2.4 (salinomycin) to 1302 (apramycin) μgkg(-1).
authors.affiliation: Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Panepistimiopolis Zographou, 15771 Athens, Greece.
authors.forename: Marilena E
authors.initials: ME
authors.lastname: Dasenaki
authors.affiliation: Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Panepistimiopolis Zographou, 15771 Athens, Greece.
authors.forename: Christina S
authors.initials: CS
authors.lastname: Michali
authors.affiliation: Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Panepistimiopolis Zographou, 15771 Athens, Greece. Electronic address: ntho@chem.uoa.gr.
authors.forename: Nikolaos S
authors.initials: NS
authors.lastname: Thomaidis
mesh_terms: D000617:Aminoglycosides / Q000032:analysis* / Q000737:chemistry; D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis* / Q000737:chemistry; D001964:Bromhexine / Q000032:analysis; D002138:Calibration; D002417:Cattle; D002853:Chromatography, Liquid / Q000379:methods; D004350:Drug Residues / Q000032:analysis* / Q000737:chemistry; D057927:Hydrophobic and Hydrophilic Interactions; D007612:Kanamycin / Q000032:analysis; D009132:Muscles / Q000737:chemistry*; D009328:Nebramycin / Q000031:analogs & derivatives / Q000032:analysis; D011714:Pyrans / Q000032:analysis; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry / Q000379:methods*; D019155:Veterinary Drugs / Q000032:analysis* / Q000737:chemistry / Q000145:classification*; D000095662:Polyether Polyketides
chemical_list: D000617:Aminoglycosides; D000900:Anti-Bacterial Agents; D001964:Bromhexine; D007612:Kanamycin; D009328:Nebramycin; D011714:Pyrans; D019155:Veterinary Drugs; C011666:apramycin; C010327:salinomycin; D000095662:Polyether Polyketides
keywords: Aminoglycosides; Electrospray ionization; Food; HILIC–MS/MS; Residues; Validation