QuEChERS方法净化UPLC-MS检测猪肉中35种兽药残留

Determination of 35 Kinds of Veterinary Drugs Residues in Pork by QuEChERS Purification-UPLC-MS

[目的]建立QuEChERS方法提取和净化、超高效液相色谱串联质谱法（UPLC-MS）检测猪肉中35种兽药残留的方法。[方法]猪肉样品分别用Na2EDTA-Mcllvaine（pH 4，0）溶液和2，5％乙酸乙腈提取后，得到的溶液以NaCl和无水Na2SO4为脱水剂，-NH2为吸附剂进行净化浓缩后，在电喷雾正离子模式下，以多反应监测（ MRM）方法进行检测，基质空白加标曲线外标法进行定性和定量分析。[结果]35种兽药在0，5-50，0 ng／mL浓度范围内线性关系良好，相关系数均大于0，995，4个不同浓度添加水平的平均回收率为60％-110％，相对偏差（RSD）均小于10％，检出限（LOD，S／N=3∶1）为0，02-1，20μg／kg，定量限（LOQ，S／N=10∶1）为0，07-4，00μg／kg。[结论]该方法简单、快速、可靠、灵敏、高效，可用于猪肉中多兽药残留的分析检测和监控。

[Objective] To establish the QuEChERS purification-UPLC-MS detection method of 35 kinds of veterinary drugs residues in pork. [Method] The pork samples were extracted by Na2EDTA-Mcllvaine （pH 4.0） and 2.5%acetic acid acetonitrile respectively, the solution ob-tained was purified and concentrated by using the dehydrating agent of NaCl and anhydrous Na2SO4 and the adsorbent of -NH2, and then was detected in electrospray ionization in positive ion mode with the method of multiple reaction monitoring （MRM）, qualitative and quantitative a-nalysis was conducted by matrix spiked blank curve external standard method.[Result] The linear relations of 35 kinds of veterinary drugs were good in the range of 0.5-50.0 ng/mL concentration and the correlation coefficients were greater than 0.995, the average recovery rates of 4 different concentrations were 60%-110%, relative deviations （RSD） were less than 10%, the detection limits（LOD, S/N=3∶1） were 0.02-1.20 μg/kg, the quantitative limits （LOQ, S/N=10∶1） were 0.07-4.00 μg/kg.[Conclusion] The method is simple, rapid, relia-ble, sensitive and efficient, and can be used for the detection and monitoring of multi drug residues in pork.