凝胶渗透净化液相色谱串联质谱法测定动物源肝脏中4种β-仪器谱.PDF

凝胶渗透净化/液相色谱串联质谱法测定动物源肝脏中4种 β－激动剂的残留量 1* 2 3 1 吴淑秀 王汉卿 公茂金 杨志刚 (1．临沂出入境检验检疫局检验检疫技术中心，山东 临沂276034； 2.华中农业大学，湖北 武汉 430070，3. 山东省交通技术学院) 摘要：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（r）均大于0.999；方法的检测限和定2 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%，该方法具有净化效果良好，灵敏度高 的优点，非常适合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。 关键词：全自动凝胶渗透净化色谱仪；液相色谱-串联质谱；动物源肝脏； β－激动剂 Determination of Four β-agonists Residues in creatural Liver by Gel Permeation Chromatography Coupled with High Performance Liquid Chromatography—tandemMassSpectrometry 1 2 3 1 WUShu-xiu ,WANG Han-qing ,GONG Mao-jin ,YANG Zhi-gang (1.Inspection and Quarantine Technology Center of Linyi Exit ／Entry Inspection and Quarantine Bureau, Linyi 276034, China;2.Huazhong agricultural university,Wuhan 430070,china;3TrafficInstitute ofTechnology,ShandongProvince,linyi 266000,China.) Abstract:Amethod for the simultaneous analysis of clenbuterol、salbutamol 、ractopamine and terbutalin residues in creatural liver was developed using high performance liquid chromatography—tandemmass spectrometry(LC-MS/MS) basedongel permeation 作者简介：吴淑秀(1974-)，女，山东临沂，农艺师，主要从事农兽药药残留检测技术的研究。E-mail: wsx7883@126.com； chromatography(GPC) purification . The homogenized sample were enzyme digested by β-glucuronidase enzyme,and extracted with ammonium acetate, Further cleanup were performed on a MCX cartridge and a GCP ,The selected ion monitoring(SIM) method was used for detection and quantified by the interal standard method.The calibration curves showed good linearities for clenbuterol in the range of 0.1～10 ng/ml and for ractopamine 、salbutamol 、