超高效液相色谱-串联质谱法测定畜禽毛发中利巴韦林及其代谢物

Determination of ribavirin and its metabolites in animal hair by ultra high performance liquid chromatography-tandem mass spectrometry

建立了一种测定畜禽毛发中利巴韦林及其代谢物1H-1,2,4-三氮唑-3-甲酰胺(TCONH2)残留的检测方法。1%十二烷基硫酸钠清洗毛发,2%甲酸-甲醇(2:98,V/V)溶液提取,13C-利巴韦林(13CRBV)内标法定量,乙二胺-N-丙基硅烷(PSA)和十八烷基硅烷(C18)基质分散净化,Agilent ZORBAX SB-Aq色谱柱分离,电喷雾串联质谱多反应监测模式测定。利巴韦林和TCONH2在毛发中线性关系良好(R^2>0.99)在2,10,100μg/kg3个添加水平下利巴韦林和代谢物TCONH2的回收率分别为101.5%~108.5%和98.5%~101.5%相对标准偏差均小于7%,检出限和定量限分别为0.2μg/kg和0.5μg/kg。该方法适合于畜禽毛发中违禁抗病毒药物利巴韦林及其代谢物TCONH2的测定。

A confirmative method was developed with ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)to detect ribavirin and TCONH2 in animal hair.Using the method,hair was washed with 1%sodium dodecyl benzene sulfonate,extracted with 2%formic acid methanol solution(2:98,V/V),quantified using 13C-RBV as the internal standard,dispersed and purified with ethylamine n-propyl silane(PSA)and octadecyl silane(C18).Then the reconstituted sample solution was analyzed by UPLC-MS/MS in positive mode using Agilent ZORBAX SB-Aq column as the separation column.The recoveries of ribaverin and TCONH2 at2,10 and 100 g/kg rang from 101.5%to 108.5%and 98.5%to 101.5%,respectively.The relative standard deviation is less than 7%,and the detection limit and quantitative limit are 0.2μg/kg and 0.5μg/kg,respectively.The method is suitable for the determination of ribavirin and TCONH2 in animal hair.