QuEChERS-HILIC-MS/MS测定禽蛋中利巴韦林及其代谢物残留量

Determination of Ribavirin and Its Metabolites in Eggs by QuEChERS-HILIC-MS/MS

建立了禽蛋中利巴韦林及其主要代谢物TCONH2、RTCOOH的QuEChERS提取净化并结合HILIC-MS/MS的检测方法。禽蛋样品经乙腈提取后,利用QuEChERS净化盐包(2 g无水硫酸钠、100 mg GCB、50 mg C18)净化后,浓缩,纯水复溶,水饱和正己烷除脂,过滤膜,在HILIC模式下进行检测,并利用利巴韦林同位素内标进行定量。在优化条件下,3种物质在2.00~100μg/L范围内线性关系良好,相关系数r不低于0.99,检出限为0.146~0.763μg/kg,定量限为0.438~2.26μg/kg。空白基质加标(5.00,10.0,50.0μg/kg)回收率为71.6%~97.3%,相对标准偏差(δ_(RSD),n=6)为3.5%~8.6%。该方法操作简单快速,精确度和准确度较好,成本低,适用于禽蛋中利巴韦林及其代谢物残留量的快速定量检测。

An analytical method was developed for the determination residues of ribavirin and its metabolites 1,2,4-triazole-3-carboxamide(TCONH2),1-β-D-ribofuranosyl-1,2,4-triazole-3-carboxylic acid(RTCOOH)in eggs by QuECh ERS-HILIC-MS/MS.The samples were extracted with acetonitrile and cleanup by QuEChERS purified salt package(2 g Na_(2)SO_(4),100 mg GCB and 50 mg C18),concentrated,reconstitution by water,liposoluble substance being removed with hexane.After subnatant was ultrafiltrated,filtrate was detected by HILIC-MS/MS and used ribavirin-^13C5 as the isotopice internal standard.Under the optimized condition,three determinands showed great linearity in the range of 2.00-100μg/L,with correlation coefficients higher than 0.99.The limit of detection(LOD)was 0.146-0.763μg/kg.The quantification was 0.438-2.26μg/kg.The recovery values of determinand residues(5.00,10.00 and 50.0μg/kg)were 71.6%-97.3%,and the within-and between-run relative standard deviation(δ_(RSD),n=6)were 3.5%-8.6%.The method was simple,fast and cheap,and had good accuracy.It was suitable for rapid determination of ribavirin and its metabolites in eggs.