超高效液相色谱-串联质谱法快速测定动物源性食品中的地塞米松残留量

Rapid determination of dexamethasone residue in animal-origin foods by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  地塞米松  超高效液相色谱-串联质谱法  内标法  动物源性食品

英文关键词:dexamethasone  ultra performance liquid chromatography-tandem mass spectrometry  internal standard method  animal-origin foods

中文摘要:

      目的 建立超高效液相色谱-串联质谱法快速测定动物源性食品中地塞米松残留量的分析方法。 方法 组织样品经碱水解, 乙酸乙酯提取, 旋近干, 正己烷除脂, 20%乙腈水定容, 以0.05%甲酸水-乙腈作为流动相, Poroshell 120 EC-C18(50 mm×2.1 mm, 2.7 μm)进行色谱分离, 超高效液相色谱-串联质谱多反应监测(multiple reaction monitoring, MRM)模式测定, 内标法定量。结果 猪肝、牛肉、鸡蛋、牛奶等4种基质中地塞米松在1~20 ng/mL范围内线性良好, 相关系数r2=0.9999, 最低定量限为0.2~1 μg/kg, 平均回收率为83.2%~108.2%, RSD为2.5%~6.5%。结论 该方法简便, 快捷, 回收率好, 精密度高, 灵敏度高, 适用于快速测定动物源性食品中地塞米松的残留量。

英文摘要:

      Objective To establish a method for the determination of dexamethasone residues in animal-origin foods by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was hydrolyzed by alkali and extracted by ethyl acetate, the extraction liquid was spin dry, and purified by N-hexane, followed by 20% acetonitrile water constant volume. The mobile phase was 0.05% formic acid water-acetonitrile. Poroshell 120 EC-C18(50 mm×2.1 mm, 2.7 μm) was used for chromatography separation. Then it was determined by HPLC-MS with multiple reaction monitoring mode. Inner standard method was used for quantitative analysis. Results The dexamethasone in 4 matrices such as the pig liver, beef, egg and milk had good linear relationships in the range of 1?20 ng/mL, with correlation coefficient (r2) was 0.9999. The limits of detection (LODs) were 0.2?1 μg/kg. The recoveries were 83.2%?108.2%, with the relative standard deviations (RSD) of 2.5%?6.5%. Conclusion This method is simple, rapid, good recovery, good repeatability and high sensitivity, which is suitable for rapid determination of dexamethasone residues in animal-origin foods.