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采用凝胶渗透净化技术,建立了用高效液相色谱串联质谱法同时测定动物源肝脏中克伦特罗、沙丁胺醇、莱克多巴胺、特步它林残留量的方法。样品经β-葡萄糖苷酸酶水解后,用乙酸铵溶液提取,MCX固相萃取柱和全自动凝胶渗透净化色谱仪净化,采用选择离子监控模式(SIM)检测,内标法定量。克伦特罗在0.1~10 ng/mL、莱克多巴胺、沙丁胺醇、特布他林在1~100 ng/mL质量浓度范围内呈良好的线性关系,相关系数(r2)均大于0.999;方法的检出限和定量限分别在0.003~0.02μg/kg和0.009~0.06μg/kg之间,方法的回收率为94.7%~106.1%,相对标准偏差小于7.8%。适用于动物肝脏中克伦特罗、沙丁胺醇、莱克多巴胺、特步它林的确认和定量检测。
Gel permeation purification technology was used to establish a method for the simultaneous determination of clenbuterol, salbutamol, ractopamine and terbutaline in animal liver by high performance liquid chromatography tandem mass spectrometry. After the sample was hydrolyzed by β-glucuronidase, it was extracted with ammonium acetate solution, purified by MCX solid phase extraction column and automatic gel permeation chromatograph. The samples were determined by SIM and detected by internal standard method. The linearities of clenbuterol at 0.1 ~ 10 ng / mL, ractopamine, salbutamol and terbutaline were in the range of 1 ~ 100 ng / mL with the correlation coefficients (r2) higher than 0.999. The limit of determination and limit of quantification were between 0.003-0.02μg / kg and 0.009-0.06μg / kg, respectively. The recoveries were 94.7% -106.1% with relative standard deviations less than 7.8%. It is suitable for the confirmation and quantitative detection of clenbuterol, salbutamol, ractopamine and Xtepital in animal liver.