同位素内标-高效液相色谱串联质谱法测定乳及乳制品中13种β-受体激动剂类药物残留

Determination of 13 β-agonists in milk and milk products with isotope internal standards by high performance liquid chromatography-electrospray ionization tandem mass spectrometry

建立了乳及乳制品中13种β-受体激动剂类药物多残留的同位素内标-高效液相色谱串联质谱分析方法。样品经三氯乙酸沉淀蛋白,提取液经SupelcleanLC-SCX固相萃取柱净化后,用HPLC-MS/MS进行测定。采用AgilentEclipse Plus C18色谱柱(2.1×150 mm,3.5μm),0.1%甲酸水-乙腈流动相进行梯度洗脱,用电喷雾离子源正离子多反应监测(MRM)模式进行MS/MS检测。其中克伦特罗在0.05～5.0μg/kg线性范围内,其余12种分析物在0.25～10μg/kg线性范围内具有较好的线性关系,相关系数r>0.9988。方法检出限(LOD)为0.02～0.17μg/kg,定量限(LOQ)为0.05～0.48μg/kg。空白样品添加回收率为83.2%～102.6%,相对标准偏差为5.0%～13%。

A high performance liquid chromatography-electrospray ionization tandem mass spectrometic（HPLCMS/MS） method has been established for the simultaneous determination of 13 β-agonists in milk and milk products with isotope internal standards.Samples were deproteinized by trichloroacetic acid and cleaned up with SupelcleanLCSCX solid phase extraction（SPE） column.The separation was performed on an Agilent Eclipse Plus C18 column（2.1 ×150 mm,3.5 μm） with gradient elution using acetonitrile and water（containing 0.1% formic acid） at a flow rate of 0.3 mL/min,and determined by tandem mass spectrometry in positive ESI mode under multiple reaction monitoring（MRM） mode.The linearity of clenbuterol in the range from 0.05 μg/kg to 5.0 μg/kg and the others in the range from 0.25 μg/kg to 10.0 μg/kg had correlation coefficient greater than 0.9988.The limits of detection（LOD） of the method were from 0.02 μg/kg to 0.17 μg/kg and the limits of quantification（LOQ） were from 0.05 μg/kg to 0.48 μg/kg.The average recoveries of 13 β-agonists were in the range from 82.3% to 102.6%,with relative standard deviations from 5.0% to 13%.