液相色谱-串联质谱法同时测定畜肉中阿托品、山莨菪碱、东莨菪碱、普鲁卡因和利多卡因残留量

Simultaneous determination of anisodamine and atropine in raw meat by liquid chromatography-tandem mass spectrometry

中文关键词:  阿托品  山莨菪碱  东莨菪碱  普鲁卡因  利多卡  液相色谱-串联质谱法

英文关键词:atropine  anisodamine  scopolamine  procaine  lidoca  liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)同时定性和定量分析畜肉中的阿托品、山莨菪碱、东莨菪碱、普鲁卡因和利多卡因残留量的方法。方法 样品用磷酸盐缓冲溶液超声提取, SPE小柱净化, 经C18色谱柱以0.1%乙酸溶液和乙腈梯度洗脱, 流速0.4 mL/min, 柱温30 ℃, 采用电喷雾离子源正离子模式, 多反应监测(multiple reaction monitoring, MRM)进行检测。结果 5种化合物在0.5~50 μg/kg范围内线性关系良好, 线性相关系数均在0.999以上。在0.5、1.5、5.0 μg/kg 3个添加水平的回收率范围为83.2%~100.3%, 5种化合物方法检出限均为 0.5 μg/kg。结论 液相色谱串联质谱法可靠、灵敏、准确, 可用于畜肉中阿托品、山莨菪碱、东莨菪碱、普鲁卡因和利多卡因残留同时定性和定量分析。

英文摘要:

      Objective To establish a method for simultaneously qualitative and quantitative analysis of residues of atropine, anisodamine, scopolamine, procaine and lidocaine in livestock meat by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The sample was ultrasonically extracted with phosphate buffer solution, purified by SPE cartridge, and the gradient was eluted with a gradient of 0.1% acetic acid and acetonitrile on a C18 column at a flow rate of 0.4 mL/min and a column temperature of 30 ℃. The electrospray ion source positive ion mode and multiple reaction monitoring (MRM) were used for detection. Results The linearities of 5 compounds in the range of 0.5-50 μg/kg were good, and the linear correlation coefficients were all above 0.999. The recoveries ranged from 83.2% to 100.3% at the spikes of 0.5, 1.5, and 5.0 μg/kg, and the limits of detection of the five compounds were 0.5 μg/kg. Conclusion The developed method is precise, accurate and sensitive, which is suitable for simultaneous qualitative and quantitative analysis of atropine, anisodamine, scopolamine, procaine and lidocaine residues in raw meat.