title: Rapid method for quantification of nine sulfonamides in bovine milk using HPLC/MS/MS and without using SPE.
abstract: Sulfonamides are antimicrobial agents widely employed in animal production and their residues in food could be an important risk to human health. In the dairy industry, large quantities of milk are monitored daily for the presence of sulfonamides. A simple and low-cost extraction protocol followed by a liquid chromatographic-tandem mass spectrometry method was developed for the simultaneous detection of nine sulfonamides in whole milk. The method was validated at the maximum residue limits established by European legislation. The limits of quantification obtained for most sulfonamides were between 12.5 and 25 μg kg(-1), detection capabilities ranged from 116 to 145 μg kg(-1), and recoveries, at 100 μg kg(-1), were greater than 89±12.5%. The method was employed to analyse 100 raw whole bovine milk samples collected from dairy farms in the northwest region of Spain. All of the samples were found to be compliant, but two were positive; one for sulfadiazine and the other for sulfamethoxipyridazine.
authors.affiliation: Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Veterinary Medicine, University of Santiago de Compostela, 27002 Lugo, Spain. carolina.nebot@usc.es
authors.forename: Carolina
authors.initials: C
authors.lastname: Nebot
authors.forename: Patricia
authors.initials: P
authors.lastname: Regal
authors.forename: Jose Manuel
authors.initials: JM
authors.lastname: Miranda
authors.forename: Cristina
authors.initials: C
authors.lastname: Fente
authors.forename: Alberto
authors.initials: A
authors.lastname: Cepeda
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000737:chemistry*; D002417:Cattle; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004350:Drug Residues / Q000737:chemistry*; D005506:Food Contamination / Q000032:analysis*; D008892:Milk / Q000737:chemistry*; D013449:Sulfonamides / Q000737:chemistry*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D000900:Anti-Bacterial Agents; D013449:Sulfonamides
keywords: 2002/657/EC; 37/2010/EC; High-performance liquid chromatography; Mass spectrometry; Milk; Sulfonamides