液相色谱串联质谱法同时测定饲料中8种苯并咪唑类药物  

Simultaneous Determination of Eight Benzimidazoles in Animal Feed by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：吴银良[1] 皇甫伟国[1] 杨挺[1] 

机构地区：[1]农业部农产品质量安全监督检验测试中心(宁波),浙江宁波315040

出　　处：《分析测试学报》2010年第12期1200-1204,共5页Journal of Instrumental Analysis

基　　金：宁波市自然科学基金资助项目(2009A610183);宁波市农科院院长基金资助项目(09-12)

摘　　要：建立了同时测定饲料中8种苯并咪唑类药物（噻苯咪唑、丙硫咪唑、硫苯咪唑、苯硫氧咪唑、氟苯咪唑、甲苯咪唑、丙氧苯唑和三氯苯唑）的液相色谱串联质谱分析方法。饲料样品用酸化乙腈直接提取,提取液用甲酸溶液稀释后进行分析。分析时用XBridgeTMC18色谱柱,以甲酸溶液-乙腈体系进行梯度洗脱,MRM方式测定,基质外标法定量。8种苯并咪唑类药物均在0.02-10.0 mg.L^-1范围内呈良好的线性关系,相关系数（r2）均不低于0.990,在饲料样品中的检出限为2.1-63.0μg.kg^-1。饲料中苯并咪唑类药物在0.50、30、200 mg.kg^-13种加标水平下的回收率为84%-104%,相对标准偏差均小于10.0%。方法分析单个样品约需30 min,该方法适合饲料中8种苯并咪唑类药物的同时分析。A high performance liquid chromatography-tandem mass spectrometric（LC-MS/MS） method was developed for the determination of benzimidazoles,e.g.thiabendazole,oxfendazole,oxibendazole,mebendazole,fenbendazole,flubendazole,albendazole and triclabendazole,in animal feed.The samples were extracted with 0.5% formic acid in acetonitrile by ultrasonic extraction.The extract was analyzed by LC-MS/MS on an XBridgeTM C18 column with a mixture of 0.1% formic acid（A） and acetonitrile（B） as mobile phase.The mass spectrometer was operated in multiple reaction monitoring（MRM） mode with positive electrospray ionization.The samples were quantified with the matrix standard calibration curve method.Good linearities were obtained for eight benzimidazoles at the concentration range of 0.02-10.0 mg·L^-1 with relative coefficients（r2） not less than 0.990.The limits of detection were in the range of 2.1-63.0 μg·kg^-1.The recoveries of the eight benzimidazoles from swine mixed feed at three fortified levels of 0.50,30,200 mg·kg^-1 were in the range of 84%-104% with RSDs lower than 10.0%.The total time required for the analysis of one sample was about 30 min.The method was suitable for the determination of eight benzimidazoles in animal feed.

关 键 词：苯并咪唑类药物 液相色谱串联质谱法 饲料 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]