基于分子印迹技术检测鸡肉中16种喹诺酮药物残留

Determination of 16 Quinolone Residues in Chicken by Molecularly Imprinted Solid-Phase Extraction

建立了同时测定鸡肉中氧氟沙星、诺氟沙星、培氟沙星、环丙沙星、洛美沙星、达氟沙星、恩诺沙星、沙拉沙星、二氟沙星、吡哌酸、麻保沙星、依诺沙星、氟罗沙星、奥比沙星、尤利沙星、加替沙星16种喹诺酮类药物残留的分子印迹固相萃取(MISPE)-超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。样品均质处理后,用磷酸盐缓冲溶液提取,经MISPE柱上样,依次用水、乙腈、2%乙酸乙腈、0.1%氨水淋洗,5%氨化甲醇洗脱,用BEHC18柱分离,以乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,电喷雾正离子多反应监测模式下,外标法定量。实验对上样液、淋洗与洗脱液的条件进行优化,结果表明,16种喹诺酮类药物检出限为0.08μg/kg,定量限为0.25μg/kg;药物浓度在0.25～200μg/L范围内相关系数(r)均大于0.99;在0.25、2.5、5.0μg/kg三个添加水平下,各药物回收率为88.6%～101.9%,相对标准偏差(RSD)为2.9%～10.5%。该方法灵敏度高,操作简单、快速。

A ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)-molecularly imprinted solid-phase extraction(MISPE)method was established for the simultaneous determination of 16 quinolone drug residues(ofloxacin,norfloxacin,pefloxacin,ciprofloxacin,lomefloxacin,danofloxacin,enrofluxacin,sarafloxacin,difluoxacin pipemidic acid,marbofloxacin,enoxacin,fleroxacin,orbifloxacin,ulifloxacin,gatifloxacin).The conditions of the MISPE column of upper sample solution,leaching and eluting were optimized.The samples were extracted with phosphate buffer solution,added on the MISPE column.The column was washed by water,acetonitrile,2%acetic acid-acetonitrile and 0.1%ammonia leaching,5%ammoniated methanol elution.The analytes were separated by Acquity LC BEH C18 column with acetonitrile-0.1%formic acid for gradient elution,detected by electrospray positive ion multi-reaction monitoring(MRM)mode.The limits of detection were 0.08μg/kg and the limits of quantification were 0.25μg/kg.The linear ranges were 0.25-200μg/L,with correlation coefficients(r)greater than 0.99.At the spiked levels of 0.25,2.5 and 5.0μg/kg,the recoveries were 88.6%-101.9%,and RSDs were 2.9%-10.5%.The method is sensitive,simple and fast for the determination of 16 quinolone drug residues.