分散固相萃取结合亲水作用色谱-串联质谱法检测预混合饲料中7种抗病毒药物含量

摘要

建立了同时检测预混合饲料中7种抗病毒药物含量的分散固相萃取(QuCHERS)结合亲水作用色谱(HILIC)-串联质谱检测方法,包括了金刚烷胺、吗啉胍、金刚乙胺、阿昔洛韦、利巴韦林、更昔洛韦和奥司他韦.选择使用乙腈提取,无水MgSO4进行脱水和盐析,C18粉和丙基乙二胺(Primary secondary amine,PSA)进行样品净化.使用亲水作用液相色谱柱进行分离,流动相为0.2%甲酸和乙腈,采用梯度洗脱,三重四级杆质谱进行定性定量分析.实验结果表明,方法的最低检出限为25μg/kg,最低定量限为50μg/kg,在50~5000μg/kg范围内线性关系良好(r>0.995),添加回收率在60%~110%之间,RSD<10%,表明该方法具有较好的准确度与精密度.%To determine 7 antivirus in feed including amantadine,moroxydine,rimantadine,acyclovir,ribavirin, ganciclovir and oseltamivir,a QuCHERS combined with hydrophilic interaction chromatography (HILIC) -tandem mass method was established.The acetonitrile was chosen to extract the target compounds,the anhydrous magnesium sulfate was chosen to dehydrate and salt out,and the C18 powder and the primary secondary amine (PSA)were chosen to purify the sample.After centrifugation,the extract was determined by the method below. The targets was separated by the gradient elution with a HILIC column as the stationary phase and 0.2% formic acid with acetonitrile as the mobile phase.The qualification and quantification were achieved by a tandem mass spectrometry.The results showed that the LOD of the method was 25 μg/kg and the LOQ was 50 μg/kg.The linearity of the method was good in the range of 50 ~5000 μg/kg and the liner correlations were all above 0.995, and the recovery of 7 targets were between 60% ~110%,and the RSD were lower than 10%,which showed the good accuracy and precision of the method.