QuEChERS-超高效液相色谱串联质谱法测定蜂蜜中11种喹诺酮类药物残留

Determination of 11 quinolones residues in honey by QuEChERS ultra-high performance liquid chromatography tandem mass spectrometry

目的优化改进QuEChERS-超高效液相色谱串联质谱(UPLC-MS/MS)测定蜂蜜中11种喹诺酮类药物残留的方法。方法样品经均质后,对比不同的提取体系和净化条件,以及基质效应的变化,优化色谱质谱条件。结果优化改进QuEChERS-超高效液相色谱串联质谱(UPLC-MS/MS)方法,选择冰乙酸-乙腈-水体系(1∶84∶15)溶液为提取试剂,采用C18+PSA(300 mg+125 mg)混合吸附剂净化,流动相为40%甲醇-乙腈和0.1%甲酸水溶液,同时优化色谱条件,结果各目标化合物在1.0~100.0μg/L质量浓度范围内线性关系良好,相关系数r均>0.995;回收率为72.4%~107.5%,相对标准偏差(RSD)为1.9%~8.1%,11种喹诺酮类药物检出限在0.4~1.0μg/kg,定量限在1.3~3.0μg/kg。结论该方法快速经济,准确可靠,适合大批量蜂蜜样品中喹诺酮类药物残留的快速测定。

Objective To improve and perfect QuEChERS ultra-high performance liquid chromatography-electrospray tandem mass spectrometry(UPLC-MS/MS)method for the determination of 11 quinolones residues in honey samples.Methods After The homogenizing samples,the different extraction systems,purification conditions and changes of matrix effect were compared to optimize the chromatography and mass spectrometry conditions.Results The QuEChERS UPLC-MS/MS method was optimized and improved.The glacial acetic acid acetonitrile buffer system(1∶84∶15)solution was selected as the extraction reagent,and C18+PSA(300 mg+125 mg)mixed adsorbent was used for purification.The mobile phase was 40%methanol acetonitrile-0.1%formic acid aqueous solution.At the same time,the chromatographic conditions were optimized;the target compounds showed good linearity within the mass concentration range of 1.0-100.0μg/L with all correlation coefficients more than 0.995.The recoveries were in the range of 72.4%-107.5%at 3 levels,and the relative standard deviation was 1.9%-8.1%.The limits of detection for 11 quinolones residues were 0.4-1.0μg/kg,and the limits of quantitation were 1.3-3.0μg/kg.Conclusion The established method is rapid and economical,accurate and reliable,which is suitable for rapid determination of quinolone residues in large quantities of honey samples.