液相色谱—串联质谱法测定动物源性食品中4种β_2^-受体激动剂类药物残留

Determination of Four Beta-agonists Residues in Animal Derived Foods by High Performance Liquid Chromatography-TandemMass Spectrometry

建立了动物源性食品中4种β2-受体激动剂克伦特罗、莱克多巴胺、沙丁胺醇和特布他林的高效液相色谱—串联质谱测定方法。样品经5%的三氯乙酸酸解提取,Waters Oasis MCX固相萃取柱净化,然后用Aglient ZORBAXSB-Aq(3.5μm,3.0 mm×100 mm)色谱柱分离,以0.1%甲酸乙腈溶液和0.1%甲酸水溶液为流动相进行梯度洗脱,基质匹配标准溶液内标法定量。结果表明,4种β2-受体激动剂在质量浓度1.0~100 g/L内呈良好的线性关系,相关系数R均大于0.995 0;检出限(S/N≥3)均为0.1μg/kg,定量下限(S/N≥10)为0.25 g/kg,在0.5,2,5μg/kg3个质量分数添加水平,回收率在81%~108%,相对标准偏差在1.3%~9.4%。方法灵敏度高、定性准确可用于各种动物源性食品中4种β2-受体激动剂残留的快速检测。

A high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） method is established for the determination of clenbuterol,ractopamine,salbutamol and turbutalin in animal derived foods.The samples are acid hydrolyzed and extracted with 5% trichloracetic acid in water,and then cleaned up by Waters Oasis MCX solid phase extraction cartridges.The separation of 4 β 2-agonists is performed on an Agilent ZORBAX SB-Aq（3.5 μm,3.0 mm×100 mm） chromatographic column and the gradient elution solvent of acetonitrile（containing 0.1% formic acid） and water（containing 0.1% formic acid） at a flow rate of 0.6 mL/min.The method is quantified by the matrix-matched internal standard method.The linear ranges of 4 β 2-agonists are 1.0-100 μg/L,the coefficient of correlation is not less than 0.995.The limit of detection（S/N≥3） for each compound is 0.1 μg/kg,and the limit of quantification（S/N≥10） is 0.25 μg/kg.The recoveries of each compound in the spiked samples at three levels 0.5,2,5 μg/kg are in the range of 81%-108%,and the relative standard deviations are in the range of 1.3%-9.4%.The method is easy,fast,sensitive,and suitable for confirmation and quantification of 4 β 2-agonists in animal derived foods.