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    全自动固相萃取-液相色谱-串联质谱法测定鸡肉中7种抗病毒药物残留量

    Determination of 7 Antiviral Drugs Residues in Chicken by Automatic Solid Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry

    • 摘要: 采用全自动固相萃取-液相色谱-串联质谱法快速测定鸡肉中金刚烷胺、金刚乙胺、美金刚、阿昔洛韦、吗啉胍、咪喹莫特和奥司他韦等7种抗病毒药物的残留量。样品用体积比为1:1的乙腈-1%(质量分数)三氯乙酸溶液的混合液提取,经全自动固相萃取仪净化,以Hilic Plus亲水色谱柱为固定相,以不同体积比的甲醇和0.1%(体积分数)甲酸溶液的混合液为流动相进行梯度洗脱,采用同位素内标法定量分析。结果表明:7种抗病毒药物的质量浓度均在1.0~20 μg·L-1内与其定量离子与内标的峰面积的比值呈线性关系,检出限(3S/N)为0.03~0.3 μg·kg-1。按标准加入法进行回收试验,回收率为75.7%~105%,测定值的相对标准偏差(n=6)均小于5.0%。与国家标准及行业标准相比,方法在保证高提取率的前提下实现了仪器自动化,且避免了试验人员过多接触有机试剂。

       

      Abstract: Automatic solid phase extraction-liquid chromatography-tandem mass spectrometry (automatic-SPE-LC-MS/MS) was applied to rapid determination of the 7 antiviral drugs (induding amantadine, rimantadine, memantine, acyclovir, moroxydine, imiquimod and oseltamivir) residues in chicken. The sample was extracted with a mixture of acetonitrile-1% (mass fraction) trichloroacetic acid solution at volume ratio of 1:1, and purified by automatic-SPE system. The chromatographic separation was performed by using Hilic Plus hydrophilic chromatographic column as stationary phase, and the mixtures of methanol and 0.1% (φ) formic acid solution at different volume ratios as mobile phase for gradient elution. Isotope internal standard method was used for quantitative analysis. It was showed that linear relationships between peak area ratio of quantitative ion to internal standard and mass concentration of the 7 antiviral drugs were found in the same range of 1.0-20 μg·L-1, with detection limits (3S/N) in the range of 0.03-0.3 μg·kg-1. Test for recovery was made by standard addition method, giving results in the range of 75.7%-105%, and RSDs (n=6) of the determined values were less than 5.0%. Compared with national standard and industry standard, this method achieved automation of instrument on the premise of high extraction efficiency, and protected the experimental personnel from being exposed to organic reagents.

       

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