一站式QuEChERS法结合UPLC-MS/MS测定动物性食品中18种β-受体激动剂残留

One Stop QuEChERS Method Combined with UPLC-MS/MS for the Determination of 18 Species in Animal Food β-Receptor Agonist Residue

目的:建立一站式QuEChERS自动提取、净化前处理系统,结合超高效液相色谱-串联质谱同时测定动物性食品中18种β-受体激动剂残留的检测方法。方法:试样加入0.2 mol·L^(-1)乙酸铵缓冲液,以β-葡萄糖醛甙酶/芳基硫酸酯酶酶解,经QuEChERS自动样品处理系统提取及净化,采用WATERS五氟苯基柱色谱柱(50 mm×3.0 mm,2.5 μm),甲酸水溶液(0.1%)和甲酸乙腈溶液(0.1%)作为液相色谱流动相梯度洗脱,串联质谱电喷雾ESI+模式,多反应监测模式测定,内标法定量。结果:18种β-受体激动剂在0.1~20.0 ng·mL^(-1)浓度范围内线性相关系数均大于0.995 5,检测限在0.025~0.100 μg·kg^(-1),阴性样品中3个水平的加标回收率为76.5%~106.8%,相对标准偏差在0.2%~3.8%(n=6)。结论:该方法安全、准确、高效,可用于大批量、快速检测动物性食品中18种β-受体激动剂残留,为建立QuEChERS法前处理方法提供依据。

Objective:To Establish a one-stop QuEChERS automatic extraction and purification pre-treatment system,combined with ultra-high performance liquid chromatography tandem mass spectrometry to simultaneously determine the residues of 18β-receptor agonists in animal food.Method:Add 0.2 mol·L^(-1) ammonium acetate buffer to the sample,andβ-Glucosidase/aryl sulfatase enzymolysis was extracted and purified by the QuEChERS automatic sample processing system.WATERS pentafluorophenyl column chromatography column(50 mm×3.0 mm,2.5μm),formic acid aqueous solution(0.1%)and formic acid acetonitrile solution(0.1%)were used as the liquid chromatography mobile phase for gradient elution,tandem mass spectrometry electrospray ESI+mode,multiple reaction monitoring mode for determination,and internal standard method for quantification.Result:The linear correlation coefficients of 18 typesβ-receptor agonists within the concentration range of 0.1~20.0 ng·mL^(-1) are all greater than 0.9955,and the detection limit is between 0.025~0.100μg·kg^(-1).The spiked recovery rates of three levels in negative samples are 76.5%~106.8%,and the relative standard deviation is 0.2%~3.8%(n=6).Conclusion:This method is safe,accurate,and efficient,and can be used for the rapid detection of 18β-receptor agonist residues in animal food in large quantities,providing a basis for establishing a QuEChERS pre-treatment method.