超高效液相色谱-串联质谱法同时测定鸡肉中43种兽药残留

Determination of 43 kinds of veterinary drug residues in chicken meat by ultra performance liquid chromatography tandem mass spectrometry

中文关键词:  正负离子切换  超高效液相色谱-串联质谱法  鸡肉  同时测定  兽药残留

英文关键词:ion switching  ultra performance liquid chromatography-tandem mass spectrometry  chicken  simultaneous determination  veterinary drug residues

中文摘要:

      目的 建立正负离子切换-超高效液相色谱-串联质谱法同时测定鸡肉中43种兽药残留量的分析方法。方法 鸡肉样品经甲酸提取液涡旋提取, 固相萃取净化, 10 mmol/L甲酸铵稀释, ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm, 1.8 μm)色谱柱分离, 以0.05%甲酸溶液和0.05%乙腈进行梯度洗脱, 正离子多反应监测39种兽药, 负离子多反应检测4种兽药, 外标法定量测定药物的含量。结果 43种兽药定量限为5 μg/kg, 标准曲线在0.4~100.0 ng/mL范围内均呈良好的线性关系。在空白鸡肉中3个不同添加水平下, 平均回收率为60%~120%之间, 变异系数为0.7%~12%。结论 该方法准确、快速、灵敏、稳定, 适合作为鸡肉中43种兽药残留量的测定。

英文摘要:

      Objective To establish a method for simultaneous determination of 43 kinds of veterinary drug residues in chicken by ion switching-ultra performance liquid chromatography tandem mass spectrometry. Methods Chicken samples were extracted by eddy extraction of formic acid extract, purified by solid phase extraction, diluted by 10 mmol/L ammonium formate, and separated by ACQUITY UPLC HSS T3 column (2.1 mm×100 mm, 1.8 μm), gradient elution with 0.05% formic acid solution and 0.05% acetonitrile. Thirty-nine kinds of veterinary drugs were monitored by positive ion multi-reaction, 4 kinds of veterinary drugs were monitored by negative ion multi-reaction, and all the 43 kinds of drug residues were quantitatively determined by external standard method. Results The limits of quantitative of 43 veterinary drugs were 5 μg/kg, and the standard curve showed a good linear relationship in the range of 0.4-100.0 ng/mL. The recoveries at 3 different levels in the blank chicken were 60%-120%, with the variable coefficient of 0.7%-12%. Conclusion This method is accurate, rapid, sensitive and stable, which is suitable for the determination of 43 kinds of veterinary drug residues in chicken.