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

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 (R) MCX cartridges, and analyzed by LC-MS/MS on an Acquity UPLC (R) BEH C-18 column with gradient elution. The method allows such multi-analyte measurements within a 13 min 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 (CC alpha), detection capability (CC beta), recovery, precision, linearity and stability. For compounds which have MRLs in bovine milk, the CC alpha values fall into a range from 11 to 115 mu g/kg, and the ccp values fall within a range of 12-125 mu g/kg. For compounds which have not MRLs in bovine milk, the CC alpha values fall into a range from 0.01 to 0.08 mu g/kg, and the CC beta values fall within a range of 0.02-0.11 mu g/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. (C) 2014 Elsevier B.V. All rights reserved.