超高效液相色谱-串联质谱法分析鸡蛋中利巴韦林及其代谢物残留

发布时间：2018-01-25 00:02

本文关键词： 超高效液相色谱-串联质谱利巴韦林及其代谢物鸡蛋　出处：《分析化学》2016年06期 　论文类型：期刊论文

【摘要】：建立了超高效液相色谱-串联质谱法同时快速测定鸡蛋中利巴韦林及其两种主要代谢物TCONH2和RTCOOH的分析检测方法。样品采用乙腈-水(9∶1,V/V)提取,乙腈饱和正己烷除脂,C18结合GCB进行固相分散萃取除杂,Agilent ZORBAX SB-Aq色谱柱(100 mm×3.0 mm,1.8μm)分离,超高效液相色谱-串联质谱测定。结果表明:利巴韦林、TCONH_2和RTCOOH分别在2.0~200μg/L,0.5~200μg/L,5.0~200μg/L浓度范围内,线性良好,相关系数R20.99,检出限分别为0.54,0.09和1.54μg/L,定量限分别为1.79,0.31和5.13μg/L。在5.0,10.0和50.0μg/L加标水平下,利巴韦林和RTCOOH回收率分别为96.1%~99.6%和42.9%~58.3%;在0.5,2.0和5.0μg/L加标水平下,TCONH2的回收率为75.9%~106.7%,相对标准偏差均为4.2%~12.7%。实际样品测定结果表明,本方法操作简单、快速、准确,能够满足鸡蛋中利巴韦林及其两种主要代谢物的分析检测。
[Abstract]:A method for the simultaneous determination of ribavirin and its two main metabolites, TCONH2 and RTCOOH, in eggs by ultra-high performance liquid chromatography-tandem mass spectrometry was established. The samples were determined by acetonitrile-water (acetonitrile-water). 9:1. V / V) extraction, acetonitrile saturated n-hexane degreasing C18 combined with GCB solid phase dispersion extraction to remove impurities. Agilent ZORBAX SB-Aq column (100mm 脳 3.0mm, 1.8 渭 m). The results of ultrahigh performance liquid chromatography-tandem mass spectrometry showed that the RTCOOH and TCONH2 of ribavirin were 200 渭 g / L and 0.5 渭 g / L, respectively. In the concentration range of 5.0 渭 g / L, the linearity was good, the correlation coefficient was R 20.99, the detection limits were 0.54 渭 g / L and 1.54 渭 g / L, and the quantitative limits were 1.79, respectively. 0.31 渭 g / L and 5.13 渭 g / L, respectively, at 5.0 渭 g / L and 50.0 渭 g / L, respectively. The recoveries of ribavirin and RTCOOH were 96.1% and 42.9%, respectively. The recoveries of TCONH2 were 75.9% and 106.7% at the standard levels of 0.5 渭 g / L and 5.0 渭 g / L. The results showed that the method was simple, rapid and accurate, and could be used for the determination of ribavirin and its two main metabolites in eggs.
【作者单位】：中国农业科学院农业质量标准与检测技术研究所农业部农产品质量安全重点实验室;南京农业大学国家肉品质量安全控制工程技术研究中心;
【基金】：“十二五”国家科技支撑计划项目(No.2012BAD28B03) 中国农业科学院科技创新工程项目资助~~
【分类号】：O657.63;TS253.7
【正文快照】： 1引言我国是禽蛋生产和消费大国,禽蛋产量多年来位居世界第一。禽类养殖过程中禽流感以及一些病毒性疾病一直是困扰养殖户的头等问题,为了减少损失,人用抗病毒药物利巴韦林曾被用于兽医临床用途。利巴韦林(1-β-D-ribofuranosyl-1,2,4-triazole-3-carboxamide)是一种人工合成

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