山羊组织中硝唑尼特代谢产物的液相色谱-串联质谱检测  

Determination of nitazoxanide metabolites in goat tissue by high performance liquid chromatography-tandem mass spectrometry

作　　者：辛瑞祥[1,2] 赵占中[1] 张丽芳[1] 王霄旸[1] 江善祥[2] 薛飞群[1] 

机构地区：[1]中国农业科学院上海兽医研究所兽药安全评价与兽药残留研究重点开放实验室农业部动物寄生虫病学重点实验室,上海200241 [2]南京农业大学动物医学院,江苏南京210095

出　　处：《中国兽医科学》2010年第3期302-306,共5页Chinese Veterinary Science

基　　金：上海市科委成果转化项目(083919n1100)

摘　　要：以替唑尼特为检测对象,建立了一种检测山羊组织中替唑尼特残留的液相色谱-串联质谱分析方法。样品经正己烷脱脂、乙腈提取,收集提取液于60℃水浴氮气吹干,乙腈溶解,经0.22μm微孔滤膜过滤后,采用多反应监测模式进行分析。结果显示,对于肝样品,替唑尼特在0.25～25μg/kg范围内线性关系良好(r2>0.99),检测限和定量限分别为0.1μg/kg和0.25μg/kg;对于肾、肌肉、脂肪样品,替唑尼特在0.1～25μg/kg范围内线性关系良好(r2>0.99),检测限和定量限依次为0.05μg/kg,0.1μg/kg;0.025μg/kg,0.05μg/kg;0.025μg/kg,0.05μg/kg。结果表明,该方法操作简单,灵敏度高,适用于山羊组织中替唑尼特残留量的检测。A sensitive and specific method for the determination of tizoxanide residues in goat tissue by liquid chromatography-tandem mass spectrometry（LC-MS/MS） was developed with tizoxanide as target substance.Tissue samples were degreased by N-hexane and extracted acetonitrile.The extracts were dried by nitrogen gas then redissolved in acetonitrile,filtered through 0.22μm micropore film and directly injected into the LC-MS/MS system and detected by the multiple reaction monitoring mode.In result,for the liver samples,the calibration curves were linear（r^2〉0.99） in the range from 0.25 to 25μg/kg.Limit of detection（LOD） and limit of quantitation（LOQ） were 0.1 and 0.25μg/kg,respectively.For kidney,muscle and fat samples of goat,the calibration curves were linear （r^2〉0.99） in the range from 0.1 to 25μg/kg.LOD and LOQ separately were 0.05 and 0.1μg/kg,0.025 and 0.05μg/kg,0.025 and 0.05μg/kg,respectively.The results showed that the developed method was simple and sensitive,which could be used to determine tizoxanide residues in goat tissue.

关 键 词：液相色谱-串联质谱法 替唑尼特 山羊组织 测定 

分 类 号：S859.84[农业科学—临床兽医学]