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

Determination of 7 Antivirus in Feed by QuCHERS Combined with Hydrophilic Interaction Chromatography- Tandem Mass Spectrometry

关键词:  7种抗病毒药物  分散固相萃取  亲水作用色谱  串联质谱法  

Key words:  7 antivirus  QuCHERS  HILIC  Tandem mass spectrometry  

摘要:

建立了同时检测饲料中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。将离心后的上清液以如下方法进行上机检测：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,采用梯度程序进行洗脱,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25 μg/kg,最低定量限为50 μg/kg,在50～5000 μg/kg范围内线性关系良好(r >0.995),添加回收率在60%～110％,RSD＜10％,表明该方法具有较好的准确度与精密度。

Abstract:

To determine 7 antivirus in feed include 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 ~ 5000μg/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.