分散固相萃取-液相色谱-串联质谱法同时测定鸡蛋中7种抗病毒类药物和利巴韦林代谢物残留量

Simultaneous determination of 7 kinds of antiviral drugs and ribavirin metabolite residues in eggs by dispersive solid phase extraction coupled with liquid chromatography-tandem mass spectrometry

中文关键词:  鸡蛋  抗病毒类药物  分散固相萃取  液相色谱-串联质谱法  残留

英文关键词:egg  antiviral drugs  dispersive solid phase extraction  liquid chromatography-tandem mass spectrometry  residues

中文摘要:

      目的 建立液相色谱-串联质谱法同时测定鸡蛋中7种抗病毒类药物和利巴韦林代谢物1H-1,2,4-三氮唑-3-甲酰胺(1H-1,2,4-triazole-3-formamide, TCONH2)残留量的分析方法。方法 匀质后的鸡蛋样品用1%乙酸乙腈提取, 提取液用N-丙基乙二胺(primary secondary amine, PSA)和C18填料进行净化, 净化液吹干复溶后进行上机测定, 选用ZORBAX SB-Aq色谱柱(100 mm×3.0 mm, 1.8 μm), 以0.1%甲酸溶液和甲醇作为流动相进行梯度洗脱, 8种化合物在正离子模式下进行监测, 内标法定量。结果 8种化合物在各自浓度范围内呈良好线性关系, 相关系数(r2)均高于0.9970, 方法检出限和定量限分别在0.03~1.50 μg/kg和0.10~5.00 μg/kg范围之间。8种化合物在低、中和高3档添加浓度水平下平均添加回收率在94.8%~108.0%之间, 批内相对标准偏差为1.8%~8.2%, 批间相对标准偏差为3.1%~5.6%。结论 该方法简单、准确、灵敏度好, 适用于鸡蛋样品中抗病毒类药物的同时分析。

英文摘要:

      Objective To establish an analytical method for simultaneous determination of 7 kinds of antiviral drugs and 1H-1,2,4-triazole-3-formamide (TCONH2) residues in eggs by liquid chromatography-tandem mass spectrometry. Methods The homogenized egg samples were extracted with 1% acetic acid acetonitrile, and the extract was purified with primary secondary amine (PSA) and C18 filler, the purified solution was dried, re-dissolved, and measured on a ZORBAX SB-Aq chromatographic column (100 mm×3.0 mm, 1.8 μm) using 0.1% formic acid solution and methanol as the mobile phase, and 8 kinds of compounds were monitored in positive ion mode and quantified by internal standard method. Results The 8 kinds of compounds showed good linear relationships within the respective concentration ranges, with the correlation coefficients (r2) higher than 0.9970, and the limits of detection and limits of quantitation of the method were in the range of 0.03?1.50 μg/kg and 0.10?5.00 μg/kg, respectively. The average recoveries of the 8 kinds of compounds at the low, medium, and high spiked concentrations were 94.8%?108.0%, with the intra-assay relative standard deviations of 1.8%?8.2%, and the inter-assay relative standard deviations of 3.1%?5.6%. Conclusion This method is simple, accurate and sensitive, and suitable for simultaneous analysis of antiviral drugs in egg samples.