摘要
建立了动物源性食品中阿莫西林和多粘菌素E残留检测的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。组织样品经三氯乙酸溶液提取,同时用乙酸铅沉淀蛋白,经正己烷除脂后,再用HLB固相萃取柱净化,浓缩后用超高效液相色谱-串联质谱仪检测,以基质匹配标准溶液定量。结果表明,阿莫西林和多粘菌素E的检出限(LOD,S/N>3)分别为6、15μg/kg,定量下限(LOQ,S/N>10)分别为20、50μg/kg。以猪肉、猪肝、猪肾和脂肪空白样品进行加标回收实验,阿莫西林、多粘菌素E的回收率分别为76%～96%和74%～92%,批内和批间相对标准偏差均小于10%。方法应用于阿莫西林和多粘菌素E复方制剂的残留消除实验,并根据实验结果计算了药物的休药期。结果证明,该法前处理简单易行,稳定性好,适用于大量样品中阿莫西林和多粘菌素E残留的同时检测。
An ultra performance liquid chromatography-tandem mass spectrometric method（UPLC-MS/MS） was established for the simultaneous determination of amoxicillin and polymyxin E residues in animal-derived food.Mass spectrometric study on amoxicillin and polymyxin E was performed,and UPLC-MS/MS conditions were optimized.Samples were extracted with trichloroacetic acid solution.The protein was precipitated with lead acetate and the fat was removed with hexane.The other impurities were removed with HLB solid phase extraction cartridge.After concentration,the analytes were detected by UPLC-MS/MS and quantified with the matrix-matched standard.The limits of detection（LOD,S/N3） for amoxicillin and polymyxin E were 6 μg/kg and 15 μg/kg,and the limits of quantitation（LOQ,S/N10） were 20 μg/kg and 50 μg/kg,respectively.The average recoveries at three spiked concentrations in muscle,liver,kidney and fat were 76%-96% for amoxicillin and 74%-92% for polymyxin E with RSDs less than 10%.Furthermore,this method was applied in the determination of amoxicillin and polymyxin E residues in swine muscle,liver,kidney and fat for elimination study,and the withdraw times were caculated on the basis of the result.The result indicated that the method was simple,rebust and was suitable for the simultaneous quantitative detection of amoxicillin and polymyxin E residues in animal-derived food.
出处
《分析测试学报》
CAS
CSCD
北大核心
2011年第8期863-867,共5页
Journal of Instrumental Analysis
基金
"十一五"国家科技支撑计划资助项目(2009BADB7B05)
