title: Development and validation of an ultra high performance liquid chromatography tandem mass spectrometry method for simultaneous determination of sulfonamides, quinolones and benzimidazoles in bovine milk.
abstract: A simple, sensitive and reliable analytical method was developed for the simultaneous determination of 38 veterinary drugs (18 sulfonamides, 11 quinolones and 9 benzimidazoles) and 8 metabolites of benzimidazoles in bovine milk by ultra high performance liquid chromatography-positive electrospray ionization tandem mass spectrometry (UHPLC-ESI-MS/MS). Samples were extracted with acidified acetonitrile, cleaned up with Oasis(®) MCX cartridges, and analyzed by LC-MS/MS on an Acquity UPLC(®) BEH C18 column with gradient elution. The method allows such multi-analyte measurements within a 13min runtime while the specificity is ensured through the MRM acquisition mode. The method was validated according to the European Commission Decision 2002/657/EC determining specificity, decision limit (CCα), detection capability (CCβ), recovery, precision, linearity and stability. For compounds which have MRLs in bovine milk, the CCα values fall into a range from 11 to 115μg/kg, and the CCβ values fall within a range of 12-125μg/kg. For compounds which have not MRLs in bovine milk, the CCα values fall into a range from 0.01 to 0.08μg/kg, and the CCβ values fall within a range of 0.02-0.11μg/kg. The mean recoveries of the 46 analytes were between 87 and 119%. The calculated RSD values of repeatability and within-laboratory reproducibility experiments were below 11% and 15% for the 46 compounds, respectively. The method was demonstrated to be suitable for the simultaneous determination of sulfonamides, quinolones and benzimidazoles in bovine milk.
authors.affiliation: Beijing Key Laboratory of Traditional Chinese Veterinary Medicine, College of Animal Science and Technology, Beijing University of Agriculture, Beijing 102206, PR China.
authors.forename: Xiao-Lin
authors.initials: XL
authors.lastname: Hou
authors.affiliation: Ningbo Academy of Agricultural Science, Ningbo 315040, PR China.
authors.forename: Guo
authors.initials: G
authors.lastname: Chen
authors.affiliation: Yinzhou Agricultural Information and Agricultural Products Quality Inspection Service Center, Ningbo 315100, PR China.
authors.forename: Li
authors.initials: L
authors.lastname: Zhu
authors.affiliation: Ningbo Academy of Agricultural Science, Ningbo 315040, PR China.
authors.forename: Ting
authors.initials: T
authors.lastname: Yang
authors.affiliation: Ningbo Academy of Agricultural Science, Ningbo 315040, PR China.
authors.forename: Jian
authors.initials: J
authors.lastname: Zhao
authors.affiliation: Beijing Key Laboratory of Traditional Chinese Veterinary Medicine, College of Animal Science and Technology, Beijing University of Agriculture, Beijing 102206, PR China.
authors.forename: Lei
authors.initials: L
authors.lastname: Wang
authors.affiliation: Ningbo Academy of Agricultural Science, Ningbo 315040, PR China. Electronic address: wupaddyfield@sina.com.
authors.forename: Yin-Liang
authors.initials: YL
authors.lastname: Wu
mesh_terms: D000818:Animals; D000871:Anthelmintics / Q000032:analysis*; D000900:Anti-Bacterial Agents / Q000032:analysis*; D001562:Benzimidazoles / Q000032:analysis*; D002417:Cattle; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D008892:Milk / Q000737:chemistry*; D015363:Quinolones / Q000032:analysis*; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D013449:Sulfonamides / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D000871:Anthelmintics; D000900:Anti-Bacterial Agents; D001562:Benzimidazoles; D015363:Quinolones; D013449:Sulfonamides
keywords: Benzimidazoles; LC–MS/MS; Milk; Quinolones; Sulfonamides