超高效液相色谱-串联质谱法同时检测鸡蛋中24种β-受体阻滞剂类药物

Determination of 24 kinds of β-blockers in eggs by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  鸡蛋  超高效液相色谱-串联质谱法  β-受体阻滞剂

英文关键词:eggs  ultra performance liquid chromatography-tandem mass spectrometry  β-blockers

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时检测鸡蛋中24种β-受体阻滞剂类药物的方法。方法 使用80%乙腈水溶液提取目标物, QuEChERS法对提取液进行净化, 乙腈饱和正己烷除脂, 经Waters ACQUITY UPLC BEH C18 (2.1 mm×100 mm, 1.7 μm)色谱柱分离, 以0.1%甲酸水溶液和乙腈作为流动相, 进行梯度洗脱。采用电喷雾离子源正离子电离模式, 使用多反应监测模式进行定量分析, 外标法定量。结果 鸡蛋基质中24种β-受体阻滞剂在考察浓度范围内呈良好的线性关系(r≥0.9963), 当称样量为1 g(精确至0.001 g), 定容体积为2 mL时, 方法检出限为3 μg/kg, 定量限为10 μg/kg, 平均加标回收率为63.6%~108.0%, 相对标准偏差(n=6)为0.9%~7.4%。结论 该方法操作简单, 回收率高, 灵敏度高, 重现性好, 可为日常及体育赛事中鲜鸡蛋中β-受体阻滞剂残留分析提供技术参考。

英文摘要:

      Objective To establish a method for the simultaneous determination of 24 kinds of β-blockers in eggs by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The 80% acetonitrile aqueous solution was used as extraction solvent, QuEChERS was used as purification method, acetonitrile-saturated n-hexane was used for degreasing, 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 ionization mode was spray positive ion mode, and quantitative analysis was performed using multiple reaction monitoring mode. The quantitative method was external standard. Results The 24 kinds of β-blockers in eggs showed a good linear relationship (r≥0.9963) in the concentration range. When the sample weight was 1 g (accurate to 0.001 g) and the final volume was 2 mL, the limit of detection was 3 μg/kg, and the limit of quantitation was 10 μg/kg. The average recoveries were 63.6%-108.0%, and the relative standard deviations (n=6) were 0.9%–7.4%. Conclusion This method has the advantages of simple operation, high accuracy, high sensitivity and good reproducibility, and can provide technical reference for the analysis of β-blocker in fresh eggs in daily life and sports events.