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 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.
作者
王海燕
姜连阁
王继双
丁宏
WANG Hai-Yan;JIANG Lian-Ge;WANG Ji-Shuang;DING Hong(National Institute for Food and Drug Control,Beijing 100050,China;Heilongjiang Institute for Food and Drug Control,Harbin 150088,China)
出处
《食品安全质量检测学报》
CAS
2018年第15期4043-4049,共7页
Journal of Food Safety and Quality