液相色谱-四极杆飞行时间质谱法同时测定 动物源性食品中的5种抗病毒类药物

Simultaneous determination of 5 kinds of antivirus drug residues in animal-derived food by high performance liquid chromatography-quadrupole-time of flight mass spectrometry

中文关键词:  液相色谱-四极杆飞行时间质谱法  抗病毒类药物  动物源性食品

英文关键词:high performance liquid chromatography-quadrupole-time of flight mass spectrometry  antivirus drugs  animal-derived foods

中文摘要:

      目的 建立同时测定动物源性食品中金刚烷胺、金刚乙胺、美金刚、奥司他韦和吗啉胍5种抗病毒类药物残留的液相色谱-四极杆飞行时间质谱(liquid chromatography-quadrupole-time-of-flight mass spectrometry, HPLC-Q-TOF-MS)分析方法。方法 样品经醋酸铵缓冲溶液与乙腈提取, 采用QuEChERS方法前处理, 经C18粉、无水硫酸镁净化。HPLC采用Agilent Eclipse XDB-C18柱进行分离, 采用电喷雾正离子模式(electrospray ionization, ESI+)进行Q-TOF-MS检测, 以分子离子精确质量数提取色谱峰面积进行定量。建立5种抗病毒药物的质谱数据库, 并通过碎片离子的精确质量数推测碎片结构。结果 猪肉、鸡肉、鱼肉、牛奶中吗啉胍的定量限为5~20 μg/kg, 金刚烷胺、金刚乙胺、美金刚、奥司他韦的定量限为0.5~1 μg/kg, 所有化合物线性相关系数r>0.99。在低、中、高3个加标水平下, 化合物回收率在72.5 %~115.5 %之间, 相对标准偏差在1.2 %~9.6 %之间(n=6)。结论 该方法操作简单、高效, 可适用于动物源性食品中5种抗病毒药物残留的检测。

英文摘要:

      Objective To establish a method for simultaneous determination of amantadine, rimatadine, memantine, oseltamivir and moroxydine in animal-derived foods by high performance liquid chromatography- quadrupole-time of flight mass spectrometry (HPLC-Q-TOF-MS). Methods Samples were extracted with acetonitrile and ammonium acetate buffer, prepared by QuEChERS method, and cleaned up by dispersive solid phase extraction using C18 sorbent and MgSO4, and then 5 kinds of antivirus drugs were separated with Agilent Eclipse XDB-C18 column by HPLC, and analyzed by Q-TOF-MS with positive electrospray ionization mode (ESI+). The quantitation analysis was carried out by extracting peak area with accurate mass, and the confirmatory analysis of target compounds were performed with qualitative fragments. An accurate mass database was established for 5 kinds of antivirus drugs, and the structures of product ions were inferred by their accurate masses. Results The results showed that the limits of quantification (LOQs) for moroxydine were in the range of 5~20 μg/kg, and LOQs for the other 4 validated compounds were in the range of 0.5~1 μg/kg in pork, chicken, fish and milk. The regression coefficients (r) were larger than 0.99. The average recoveries spiked at low, medium and high levels were in the range of 72.5 %~115.5 % with relative standard deviations (RSD) of 1.2 %~9.6 % (n=6). Conclusion The method is simple and efficient, which is suitable for the analysis of 5 kinds of antivirus drugs in animal-derived foods.