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

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 m L/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0.5~50μg/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、5.0μg/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0.5μg/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。

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 m L/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.