超高效液相色谱-串联质谱法测定动物源性食品中32种神经系统药物

Determination of 32 kinds of nervous system drugs in animal-derived foods by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  兽药  液相色谱-串联质谱  动物源性食品  PRiME HLB

英文关键词:Veterinary drugs  Liquid chromatography tandem mass spectrometry  Food of animal origin  PRiME HLB

中文摘要:

      目的:本文建立了一种应用超高效液相色谱-串联质谱仪对动物源性食品中多种β受体激动剂、兴奋剂及镇静剂类药物同时进行检测的方法。方法:考察了不同前处理条件和仪器条件对检测结果的影响,从而选出最佳解决方案。本方法以β-葡萄糖醛酸酶/芳香基硫酸酯酶进行酶解,酸性乙腈进行提取,PRiME HLB净化,用乙腈+0.1%甲酸水作为流动相,UPLC-MS/MS确证检测,外标法定量。结果:β受体激动剂类药物的检测低限可以达到0.2 μg/kg；兴奋剂、镇静剂类药物的测定低限可以达到0.5 μg/kg；麻醉剂类药物的测定低限可以达到1.0 μg/kg。肌肉中32种待测药物的相关系数均高于0.9914,回收率为62~106%,相对标准偏差为1.5~8.7%,肝脏中32种待测药物的相关系数均高于0.9916,回收率为53~110%,相对标准偏差为1.3~9.6%。结论:与传统检测方法相比,具有检测药物种类多、最低检测限低、稳定性好、简便快捷、节省试剂等优势。同时应用该方法对经过长途运输后的畜禽等动物源性食品样本进行检测分析,确定多种兽药在运输过程中的使用情况,为更好的控制运输过程中多种药物的使用提供参考。

英文摘要:

      Objective:This article established a method for the simultaneous detection of β-agonists, stimulants and sedatives in the muscles of livestock and poultry using ultra high performance liquid chromatography tandem mass spectrometry. Method:Different pretreatment conditions and instrument conditions on the detection results were investigated, and the best solution was selected.The glucuronic acid was hydrolyzed by β-lipase aryl sulfate, extracted by acidic acetonitrile and purified by PRiME HLB,using the mixture of acetonitrile and 0.1% formic acid wateras as mobile phase, confirmed by UPLC-MS/MS, and quantified by external standard method.Results:The detection limit of β-agonists was 0.2 μg/kg;the low limit of determination of stimulants and sedatives was 0.5 μg/kg;the low limit of determination of anesthetics was 1.0 μg/kg.The correlation coefficients of 32 drugs in muscle were all higher than 0.9914, the recoveries were 62 ~ 106% , the relative standard deviation was 1.5 ~ 8.7% , the correlation coefficients of 32 drugs in liver were all higher than 0.9916, the recoveries were 53 ~ 110% , the relative standard deviation was 1.3-9.6% .Conclusion:Compared with the traditional methods, the method has many advantages, such as more kinds of drugs, low detection limit, good stability, simple and convenient, reagent-saving. At the same time, the method was applied to detect and analyze the animal-derived food samples after long-distance transportation, to provide reference for better control of multi-drug use during transportation.