超高效液相色谱-串联质谱法测定动物源性食品中三种β-受体激动剂残留量

Simulataneous Determination of Three β-agonist Residues in Animal Derived Foods by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

建立了同时测定动物源性食品中3种β-受体激动剂(沙丁胺醇、莱克多巴胺和克伦特罗)残留量的超高效液相色谱-串联质谱方法 (UPLC-MS/MS)。样品经粉碎后用乙酸钠缓冲液提取,经β-盐酸葡萄糖醛苷酶-芳基硫酸酯酶水解后,用MCX阳离子交换柱净化、多反应监测(MRM)、同位素内标法定量。结果表明,3种β-受体激动剂在一定质量浓度范围(1.0~12.0μg/kg)呈现出良好的线性关系,3种β-受体激动剂的相关系数R^2>0.999;从0.5,1.0,2.0μg/kg共3个添加浓度的检测结果中可以看出,3种化合物的回收率为87.5%~117.9%,相对标准偏差(RSD)为4.6%~18.4%。

The method for the simulataneous determination of three β-agonists （salbutamol, ractompamine,clenbuterol） residues in animal derived foods is developed by ultra performance liquid chromatography-tandem mass spectrometry （UPLC- MS/MS） . The sample is extracted in acetate buffer, hydrolyzed by β-glucuronidase-arylsulfatase. The extraction is applied to a solid phase extraction MCX cartridge for cleanup,determined by MRM,quantified by internal standard method. The cali-bration curves are goog liner between the peak arears and the concentrations of 1.0-12.0 pg/kg with the correlation coefficient R2〉0.990. The average recoveries from spiked animal issues at three concentrations of 0.5, 1.0,2.0 pg/kg ranged 87.5 %- 117.9%. The relative standard deviations of intra-and inter-batch are both less than 4.6%-18.4%.