4种不同净化方法在猪肉兽药残留检测中的应用比较研究

目的 通过对猪肉中194种兽药残留的回收率和基质效应进行分析, 评价ProElut、PRiME、EMR、LipoNo 4种方式的净化效果。方法 样品采用0.1%甲酸-90%乙腈混合溶液提取后, 取上清液分别经ProElut、PRiME、EMR、LipoNo 4种不同的方式净化, 氮吹浓缩复溶后经超高效液相色谱-串联质谱法分析, 考察兽药的回收率和基质效应。结果 经4种方式净化后, 分别有84.5%、82.0%、80.0%、91.2%兽药的回收率在60%~120%之间, 回收率低于60%或高于120%的兽药数量分别是30、36、38、17种; 分别有62.9%、55.7%、83.0%、83.0%兽药的基质效应为弱基质效应, 6.2%、4.6%、3.1%、3.1%的兽药为强基质效应。结论 LipoNo处理后各类兽药平均回收率在60%~120%间比例最多, 基质效应干扰相对较小, 适用于猪肉中194种兽药残留量的测定。

Comparative study of 4 kinds of different purification methods in detection of veterinary drug residues in pork

Objective To evaluate the purification effects of 4 kinds of ProElut, PRiME, EMR and LipoNo through analyzing the recovery rates and matrix effects of 194 kinds of veterinary drug residues in pork. Methods The samples were extracted with 0.1% formic acid and 90% acetonitrile mixed solution, the supernatant was purified by 4 kinds of different methods including ProElut, PRiME, EMR and LipoNo, concentrated by nitrogen blowing, redissolved and analyzed through ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) to investigate the recovery rates and matrix effects of veterinary drugs. Results After purified by ProElut, PRiME, EMR and LipoNo, the recovery rates of 84.5%, 82.0%, 80.0% and 91.2% veterinary drugs were between 60% and 120%, respectively, the numbers of veterinary drugs with recovery rates lower than 60% or higher than 120% were 30, 36, 38 and 17, respectively; the matrix effects of 62.9%, 55.7%, 83.0% and 83.0% veterinary drugs were weak, 6.2%, 4.6%, 3.1% and 3.1% veterinary drugs had strong matrix effects, respectively. Conclusion After LipoNo treatment, the average recoveries of all kinds of veterinary drugs in the ranged from 60% to 120% are the hightest, and matrix effects interference are relatively small, which is suitable for the determination of 194 kinds of veterinary drug residues in pork.