UPLC-MS/MS测定猪肉中3种β-受体激动剂残留量

Determination of threeβ-receptor agonist residues in pork by UPLC-MS/MS

建立超高效液相色谱-三重四级杆串联质谱快速、高效检测肉制品中克伦特罗、沙丁胺醇、莱克多巴胺3种β-受体激动剂的方法。混合加标猪肉经正己烷去除油脂,异丙醇-乙酸乙酯(6∶4,V/V)提取浓缩,MCX柱富集净化,以乙腈-0.1%甲酸水溶液为流动相,用Agilent C18色谱柱进行梯度洗脱分离,多级反应监测(MRM)模式进行检测,外标法定量。3种β-受体激动剂残留量的检出限为0.3~0.4μg/kg,在5~100 ng/mL的线性范围内,相关系数R2均>0.998,平均加标回收率为81.8%~103.1%,相对标准偏差(RSDs)均<10%。因此本方法基质干扰小、灵敏度高、重复性好、定性和定量准确可靠,满足于动物源性食品中β-受体激动剂残留量的测定要求。

A rapid and efficient method for the determination of threeβ-receptor agonists of clenbuterol,salbutamol and ractopamine in meat products by ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established.The pork with mixed standards was degreased by n-hexane,extracted and concentrated by isopropanol-ethyl acetate(6∶4,V/V),enriched and purified by MCX column,gradient eluted and separated with acetonitrile-0.1%formic acid aqueous solution and Agilent C18 column,detected by multiple reaction monitoring(MRM)mode,and quantitated by external standard method.The detection limits of the threeβ-receptor agonist residues were 0.3-0.4μg/kg.In the linear range of 5-100 ng/ml,the correlation coefficients R2 were greater than 0.998.The average adding standard recovery rates were between 81.8%and 103.1%,and the relative standard deviations(RSDs)were less than 10%.The method had small matrix interference,high sensitivity,good repeatability,accurate and reliable quantitative and quantitative,which met the determination requirements ofβ-agonist residues in animal-derived foods.