超高效液相色谱质谱法快速检测动物源性食品中的四种兽药残留

doi:10.13386/j.issn1002-0306.2012.16.031

超高效液相色谱质谱法快速检测动物源性食品中的四种兽药残留

Rapid determination of four veterinary drugs residue in animal products by UPLC-MS/MS

摘要

摘要: 建立了采用超高效液相色谱串联质谱仪快速检测动物组织中甲氧苄胺嘧啶、克林霉素、泰妙菌素和吡喹酮四种药物残留的分析方法。动物组织样品经乙腈提取后,用正己烷去除脂肪等杂质,Waters Acquily UPLC BEH C18色谱柱分离,以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱,电喷雾正离子（ESI+）模式电离,液相色谱-质谱法（UPLC-MS/MS）测定。结果表明:4种药物在2.5～200μg/L范围内呈现良好的线性关系,相关系数R2均大于0.996,在此范围内添加回收率为65.8%⁹5.9%,相对标准偏差为3.2%¹3.1%,定量下限为0.5μg/kg。

Abstract: An ultra performance liquid chromatography coulped to tandem mass spectrometry (UPLC-MS/MS) method was established for the determination of trimethoprim, clindymycin, tiamulin and praziquantel residues in animal origin food. The sample was extracted with acetonitrile, purified by hexane, and detected on Waters Acquity UPLC BEH C18 column by a gradient elution using acetonitrile (A) —0.1% formic acid (B) as mobile phase with a flow rate of 0.3mL/min. The calibration curves were good linear between the peak areas and concentrations of 4 veterinaries in the range of 2.5～200μg/L, with correlation coefficients more than 0.996. The average recoveries at this concentration levels ranged from 65.8% to 95.9%, the RSD was in the range of 3.2%¹3.1%.The limits of quantification of 4 drugs in animal origin food were 0.5μg/kg.