超高效液相色谱-串联四极杆质谱法测定麻辣烫中喹诺酮类药物残留

摘要

建立了麻辣烫中14种喹诺酮类药物残留的超高效液相色谱-串联四极杆质谱(UPLC-MS/MS)检测方法.采用酸化乙腈提取麻辣烫中的喹诺酮类药物残留,提取溶液经盐析和C18固相萃取柱净化后,在电喷雾离子源中正离子模式下,采用多反应监测(MRM)方式进行测定,内标法定量.结果显示,14种喹诺酮类药物在7.5 ～ 100 μg/L范围内线性关系良好,相关系数均大于0.990.在3个不同加标水平下的平均回收率为75.4％～110.0％,相对标准偏差(n=6)为1.3％～10.1％,14种化合物的检出限和定量下限分别为0.5,1.5μg/kg.该方法操作简单、快速,净化效果好,灵敏度高,适用于麻辣烫中多种喹诺酮类药物残留的同时定性和定量检测.%An ultra performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) method was established for the determination of 14 quinolones in hotpot.Samples were extracted with acidified acetonitrile,defated with n-hexane,separated on a C1s solid phase extraction(SPE)column,and analyzed by LC-ESI-MS/MS under the positive mode with multiple reaction monitoring(MRM).The method showed good linearities for 14 quinolones over the range of 7.5-100 μg/L with correlation coefficients(r) more than 0.990.The detection limits of 14 quinolones were 0.5 μg/kg,and the quantitation limits were 1.5 μg/kg.The recoveries of all analytes in hotpot ranged from 75.4％ to 110.0％ with relative standard deviations (RSD,n =6) of 1.3％-10.1％.The method has the advantages of simplicity,rapidness,good purifying effect and sensitivity,and is suitable for the simultaneous determination of quinolones in hotpot.