超高效液相色谱-串联质谱法测定冻烤鳗中4种四环素类药物残留

建立了同时检测冻烤鳗中4种四环素类药物残留的超高效液相色谱-串联质谱法。样品采用4%高氯酸溶液提取,经HLB固相萃取柱净化,浓缩后以0.4%甲酸水溶液和甲醇作流动相进行梯度洗脱,电喷雾离子源,以正离子多反应监测模式(MRM)测定。4分钟内完成冻烤鳗中4种四环素类药物的残留检测。本方法在20~200μg/kg浓度范围内4种四环素类药物呈良好线性,其相关系数r0.9900,回收率均在72.4%~94.6%之间,相对标准偏差范围为4.6%~6.9%。土霉素、四环素、金霉素、多西环素的检测限(LOD)分别为1.55、1.48、5.91、3.11μg/kg;定量限(LOQ)分别为5.17、4.94、19.70、10.37μg/kg。本方法简便、快速、灵敏,适用于冻烤鳗中四环素类药物残留的检测。

Determination of 4 Tetracyclines residues in Frozen Roasted Eel Tissue by UPLC-MS/MS

Developed a method which could detect 4 tetracyclines residues in frozen roasted eel tissue by UPLC-MS/MS. It was extract by 4%perchloric acid solution from frozen roasted eel tissue. And then the sample solution was purified by a HLB solid phase extraction column. Take methanol-0.4%formic acid solution as mobile phase with gradient elution after the sample concentration. The detection mode was multiple reaction monitoring with positive-ion electrospray ionization. The run time for the determination of the 4 tetracyclines was only 4 minutes. This method showed a good linear relationship in the range of 20~200μg/kg for the 4 tetracyclines drug. The correlation coefficient was over 0.9900. The recoveries was 72.4%~94.6%with the relative standard deviation of 4.6%~6.9%. The limit of detection(LOD)for OTC,TC,CTC and DC were 1.55、1.48、5.91、3.11μg/kg and limit of quantitation(LOQ)were 5.17、4.94、19.70、10.37 μg/kg,respectively. The method is convenient,fast,sensitive and reproducible and it is suitable for determining OTC,TC,CTC and DC resi-dues in Frozen Roasted Eel Tissue.