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

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C_(18)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,1.8μm),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(r^(2))均高于0.9970,方法检出限和定量限分别在0.03~1.50μg/kg和0.10~5.00μg/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。

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 C_(18) filler,the purified solution was dried,re-dissolved,and measured on a ZORBAX SB-Aq chromatographic column(100 mm×3.0 mm,1.8μm)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(r^(2))higher than 0.9970,and the limits of detection and limits of quantitation of the method were in the range of 0.03‒1.50μg/kg and 0.10‒5.00μg/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.