HPLC-MS/MS测定动物源性食品中利巴韦林和金刚烷胺药物残留

Simultaneous Determination of Ribavirin and Amantadine Residues in Animal Derived Food by HPLC-MS/MS

本文建立了固相萃取净化结合液相色谱质谱联用仪同时测定动物源性食品中利巴韦林和金刚烷胺药物残留的方法,优化样品前处理和质谱条件,样品经三氯乙酸溶液提取,酸性磷酸酯酶进行酶解,混合型离子交换固相萃取小柱富集净化,氮吹浓缩,供液相色谱质谱联用仪测定。结果表明,在0.5~20μg·kg^(-1)的浓度范围内呈良好线性关系,相关系数R^(2)>0.99,检出限为1μg·kg^(-1),定量限为2μg·kg^(-1),在3个加标水平下,回收率为85%~104%,相对标准偏差在0.8%~2.4%,该方法灵敏度高、富集性好、回收率高,可用于动物源性食品中利巴韦林和金刚烷胺药物残留的测定。

In this paper,a method for simultaneous determination of ribavirin and amantadine residues in animalderived foods with solid-phase extraction and purification combined with liquid chromatography-mass spectrometry was established.The sample pretreatment and mass spectrometry conditions were optimized.The samples were extracted with trichloroacetic acid solution.Use acid phosphatase for enzymatic hydrolysis,use mixed ion exchange solid phase extraction cartridges for enrichment and purification,nitrogen blowing and concentration,for determination by liquid chromatographymass spectrometer.The results show that there is a good linear relationship in the concentration range of 0.5~20μg·kg^(-1),the correlation coefficient R^(2)>0.99,the detection limit is 1μg·kg^(-1),and the quantification limit is 2μg·kg^(-1).With a standard addition level,the recovery rate is 85%~104%,and the relative standard deviation is 0.8%~2.4%.This method has high sensitivity,good enrichment and high recovery rate.It can be used for the determination of ribavirin and amantadine residues in animal-derived foods.