动物源性食品中多种兽药残留UPLC-MS/MS分析方法的构建

Development of a UPLC-MS/MS Analysis Method for Multiple Veterinary Drug Residues in Animal-Derived Foods

利用Sin-QuEChERS Nano净化柱结合液相色谱串联质谱(UPLC-MS/MS)分析,建立了畜禽肉中27种不同极性兽药残留的快速筛查方法。通过比较Sin-QuEChERS Nano法、QuEChERS法、固相萃取法下目标物的净化效率,Sin-QuEChERS Nano法的加标回收率高于其他2种净化方法,在85%~112.5%之间。通过方法学考察表明:目标物在线性范围内均可呈现良好的线性关系,相关系数在0.9986~0.9999之间,方法检出限在0.1~1.0μg/kg,方法定量限在0.5~3.0μg/kg。在低、中、高3个水平下,目标化合物的加标回收率为85.0%~112.5%,相对标准偏差为1.6%~8.2%,与固相萃取法、QuEChERS法相比,该方法具有操作简单、检测快速、有效、可靠的特点,具有较为实际的应用价值。因此,该方法可以适用于更多种类的兽药目标化合物检测,并可用于检测其他类型的样品。

A rapid screening method for 27 different polar veterinary drug residues in livestock and poultry meat was estab-lished by using Sin-QuEChERS Nano column and liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).By compar-ing the purification efficiency of the target compound by Sin-QuEChERS Nano method,Quechers method and solid phase extraction method,the recovery rate of Sin-QuEChERS Nano method was higher than that of the other two purification methods,ranging from 85%to 112.5%.The results showed that the linear correlation of the target was good in the linear range,the correlation coeficient was 0.9986-0.9999,the detection limit was 0.1-1.0μg/kg,and the quantitative limit was 0.5-3.0μg/kg.The recoveries of target compounds were 85.0%-112.5%and RSD was 1.6%-8.2%at low,middle and high levels,Compared with the solid phase extraction method and QuEChERS method,this method has the characteristics of simple operation,rapid detection,effective and reliable,and has more practical application value.Therefore,the method can be used to detect more kinds of veterinary drug residues,and can be used todetectothertypes of samples.