食品中99种兽药的一步式提取净化体系

建立了99种禁限用兽药的一步式提取净化体系，并通过高效液相色谱-四极杆/静电场轨道阱高分辨质谱（UHPLC-Q-Orbitrap HRMS）对其效果进行了评价。该提取净化体系基于载体辅助液液萃取技术，通过一次性前处理，完成常见的理化性质差异很大的8大类共计99种兽药残留的提取、净化工作，同时结合四极杆静电场轨道阱高分辨质谱实现了99种兽药残留的一步式多残留筛查。采用此体系对样品禁限用兽药进行测定分析，结果表明，该方法对液态乳、猪肉、鱼类等食品基质具有较强的适用性，检测的99种兽药线性范围为0.001~0.1 μg/mL，定量限为0.5~20.0 μg/kg，加标回收率为60%~120%，相对标准偏差小于15%。该方法的前处理和仪器分析过程对不同理化性质的化合物的兼容性强，检测效率高，可操作性强，检出限能满足所有受试的目标物，并且大大降低了检测成本。

System of simultaneous extraction and cleaning of 99 veterinary drugs in food

We established a system for the simultaneous extraction and cleaning of 99 veterinary drugs from food by ultra-performance liquid chromatography coupled with quadrupole electrostatic field-orbital trap-high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS). The system is based on the supported liquid-liquid extraction technology through one-off pretreatment, which covers the common eight categories of physical and chemical properties, and the extraction and purification of 99 different veterinary drug residues. At the same time, the one-step multi residue screening of 99 veterinary drug residues has been realized using HRMS. The results showed that the method was suitable for extraction from milk, pork, and fish. The 99 veterinary drugs showed a good linear relationship in the concentration range of 0.001-0.1 μg/mL, the limit of quantification was 0.5-20.0 μg/kg, the average recoveries were 60%-120%, and the relative standard deviations (RSDs) were not more than 15%. The pre-processing and instrumental analysis of this method have high detection efficiency, strong maneuver ability, and strong compatibility with different physical and chemical compounds. Moreover, the detection limit can meet all the objects of the test and greatly reduce the detection cost.