Simultaneous determination of 22 cephalosporins drug residues in pork muscle using liquid chromatography-tandem mass spectrometry

摘要

A simple, sensitive and reliable analytical method was developed for the simultaneous determination of 22 common cephalosporins from the first generation to the fourth generation in pork muscle by liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method. Under the optimized extraction conditions, samples were directly purified through membrane filtration to separate all 22 cephalosporins and the critical pairs of each parent drug were completely separated. Variables affecting the LC-MS/MS were optimized to get a better separation. The excellent selectivity and sensitivity achieved in multiple reactions monitoring (MRM) mode allowed satisfactory confirmation and quantitation for the 22 cephalosporins. The linear range of the 22 cephalosporins is 0.06-100.0 mu g/L with good correlation coefficients (r(2) > 0.9920). The limits of detection (LODs) and limits of quantitation (LOQs) of these compounds were in the range 0.04-3.0 mu g/L and 0.06-10.0 mu g/kg, respectively. The average intra-day recoveries at 3 spiked levels (LOQ, 2LOQ 4LOQ) were all in the range 83.6-113.0% with RSDs (n = 6) lower than 6.5%. The method of LC-MS/MS developed in this study was initially applied to the research of 22 cephalosporins in 12 retail pork samples and proved to be accurate, sensitive, minimum sample pre-treatment, convenient and practical. (C) 2016 Elsevier B.V. All rights reserved.