多壁碳纳米管分散固相萃取结合LC-MS-MS测定鸡肉中金刚烷胺.pdf

OMID42014,Wo.28,Mo.04肉类研究中肉热品合研中分析检测MEAT RESEARCHCHINA MEAT RESEARCH CENTER多壁碳纳米管分散固相萃取结合LC-MS-MS测定鸡肉中金刚烷胺孙亚米,刘勇军2,赵健,叶宇飞,吕燕,吴银良(1.宁波市农业科学研究院,浙江宁波315040;2.中国动物疫病预防控制中心,北京100125)摘要:建立了采用多壁碳纳米管为吸附剂的分散固相萃取净化、液相色谱串联质谱测定鸡肉中金刚烷胺残留量的方法。鸡肉样品经乙酸乙腈提取后,调节pH值至11,加入75mg多壁碳纳米管进行分散固相萃取,被吸附的药物经5-0%甲酸溶液:甲醇(5:5,WV)洗脱,洗脱液过滤膜后自接进样分析。采用 Acquity UPLC BEH C1s色谱柱分离,以0.1%甲酸水溶液和甲醇作为流动相作梯度洗脱,电喷雾正电子(ESr)模式电离,多反应监测模式检测,内标法校准进行定量。金刚烷胺在0.055.0ug兀L质量浓度范围内呈良好的线性,线性相关系数均大于0.99,鸡肉样品中最低定量限为0.50ugkg。鸡肉样品中添加0.51.0gkg金刚烷胺的回收率在97.8%103.6%之间,相对标准偏差均小于10%关键词:金刚烷胺;液相色谱串联质谱法;多壁碳纳米管;分散固相萃取Determination of Amantadine in Chicken Muscle by Liquid Chromatography with Tandem Mass SpectrometryCoupled with Dispersive Solid Phase Extraction Using Multiwalled Carbon Nanotubes as AdsorbentSUN Ya-mi, LIU Yong-jun , ZHAO Jian YE Yu-fei, LU Yan, WU Yin-liang(1, Ningbo Academy of Agricultural Sciences, Ningbo 315040, China;2. The Center for Animal Disease Control and Prevention, P.R. China, Beijing 100125, China)Abstract: A simple, sensitive and reliable analytical method was developed for amantadine in chicken muscle by ultra highperformance liquid chromato raphy-positive electrospray ionisation tandem mass pectrometry(hplc-esi-ms/MS)usingdispersive solid phase extraction( PE with mul -walled carbon nanotubes(MWCNTS).Chicken muscle was extractedusing 1.0% actic acid in acetonitrile. After adjusting PH value to I l, 75 mg of MWCNTS were added to absorpt amantadineand 5.0% formic acid solution: methanol(5: 5, was used to elute the compound from the MWCNTS. The eluate wasdirectly analyzed by LC-MS-MS on an Acquity UPLC BEH Cw column with a mixture of methanol and 0.1% formicacid solution as the mobile phase. The samples were quantified with the internal standard calibration curve method. Goodlinearities were obtained for amantadine in the concentration range of.05-50 u /L with correlation coefficient more than0.999. The recoveries for amantadine in chicken muscle were 978-1036at three fortified levels(0.5, 0.75 and 1.0 ug/kg)with relative standard deviations less than 10.0%(n=3 ). The limit of quantitation was 0. 5 ug/kKey words: amantadine, LC-MS-MS; MWCNTS; dispersive solid phase extraction中图分类号:TS251.7文献标志码:A文章编号:1001-8123(2014)040014-05金刚烷胺( amantadine)最早用于抑制人类流感病毒在畜禽养殖中使用此类药物。我国农业部也于2005年发的抗病毒药,同时也是帕金森综合症的治疗药物。但金布了关于清查金刚烷胺等抗病毒药物的紧急通知刚烷胺对食用者可能产生喈睡、失眠、眩晕、抑郁、恶明令禁止金刚烷胺类抗病毒药物用于畜禽养殖业。然而、食欲减退等多种不良反应,具有一定的毒副作用目前我国畜禽饲养中滥用金刚烷胺现象依然存在,为保在畜牧养殖上,金刚烷胺主要用于鸡禽流感的预防和早障公众身体健康,急需建立动物性食品中快速、灵敏和期治疗,以及猪传染性胃肠炎的防治,但长期使用金刚准确的金刚烷胺残留量分析方法烷胺会使病毒产生耐药性,因此美国食品与药品监督管对于金刚烷胺类药物残留量的分析,在该类理局( Food and Drug Adminitration,FDA)已明确禁止药物禁止在动物生产中使用前样品主要是生物体收稿目期:2014-01-23作者简介:孙业米(1963-),女,农艺师,学士,研究方向为农产品中农兽药残留分析。E-mail:changsky(1tom.com*通信作者:吴银良(1975-)男,教授级高级工程师,博士,研究方向为农产品中农兽药残留分析。E-mail:wupaddyfieldsina.com