超高效液相色谱-串联质谱法同时测定禽蛋中6 种喹诺酮类兽药残留量及 8 种新烟碱类杀虫剂残留量

Rapid determination of 6 kinds of quinolone qesidues and 8 kinds of neonicotinoid insecticides in poultry eggs by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  禽蛋  液相色谱-串联质谱  喹诺酮类  新烟碱类

英文关键词:poultry eggs  ultra performance liquid chromatography-tandem mass spectrometry  quinolone residues  neonicotinoid insecticides

中文摘要:

      目的 建立一种超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定禽蛋中6种喹诺酮类兽药残留及8种新烟碱类杀虫剂残留的分析方法。方法 使用4% (V/V)甲酸-乙腈溶液作为提取溶剂, QuEChERS为净化方法, Waters ACQUITY UPLC BEH C18 (2.1 mm×100 mm, 1.7 μm)为色谱柱, 以乙腈-0.1%甲酸溶液作为流动相进行梯度洗脱, 柱温35 ℃, 流速0.2 mL/min。电离方式为喷雾正离子模式, 使用多反应监测模式进行定量分析。结果 14种分析物在考察浓度范围内呈良好的线性关系(R2>0.995), 方法检出限为0.3~5.0 μg/kg, 方法定量限为1~10 μg/kg, 平均加标回收率为74.8%~105.0%, 相对标准偏差为3.1%~9.5%。结论 本研究所建立的方法方便快捷、准确度高、稳定性好, 能够对禽蛋中6种喹诺酮类兽药残留及8种新烟碱类农药残留进行定量分析。

英文摘要:

      Objective To establish an analytical method for rapid determination of 6 kinds of quinolone residues and 8 kinds of neonicotinoid insecticides in poultry eggs by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The 4% (V/V) formic-acetonitrile solution was used as extraction solvent, QuEChERS was used as purification method, Waters ACQUITY UPLC BEH C18 (2.1 mm×100 mm, 1.7 μm) column was used for gradient elution with acetonitrile-0.1% formic acid solution as mobile phase. The column temperature was 35 ℃ and the flow rate was 0.2 mL/min. The ionization mode was spray positive ion mode, and quantitative analysis was performed using multiple reaction monitoring mode. Results The 14 kinds of analyte showed a good linear relationship (R2>0.995) in the concentration range. The limits of detection were 0.3–5.0 μg/kg, and the limits of quantitation were 1–10 μg/kg. The average recoveries were 74.8%~105.0%, and the relative standard deviations were 3.1%–9.5%. Conclusion This method has the advantages of simple sample pretreatment, good reproducibility and high accuracy, and can be applied to the simultaneous determination of 6 kinds of quinolone qesidues and 8 kinds of neonicotinoid insecticides in poultry eggs.