超高效液相色谱串联质谱法测定自制泡酒中的3种乌头碱

Determination of three kinds of aconitum alkaloids in self-made sparkling wine by high performance liquid chromatography-mass spectrometry

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)测定自制泡酒中的乌头碱、次乌头碱和新乌头碱的分析方法。方法自制泡酒样品经0.22μm滤膜过滤,稀释或直接进样检测分析,色谱柱为C18(50 mm×2.1 mm,1.8μm),流动相为20 mmol/L乙酸铵(0.1%甲酸)-乙腈,10 min等阶采样,质谱进行检测。结果 3种乌头碱的线性范围均为0.2~600μg/L,相关系数大于0.998,3种乌头碱的检出限分别为0.10、0.20、0.20μg/L,3种乌头碱的加标回收率为66.0%~95.0%,相对标准偏差为1.0%~5.0%。结论方法准确、灵敏、选择性强,适用于泡酒中乌头碱的检测及由乌头碱引起的食物中毒事件的诊断分析。

Objective To establish a method for the determination of aconitine,hypaconitine and neoaconitine in self-made sparkling wine by ultra performance liquid chromatography-mass spectrometry(UPLC-MS/MS).Methods The self-made sparkling wine samples were filtered by a 0.22 μm filter membrane,diluted or directly injected for detection and analysis.The chromatographic column was C18(50 mm×2.1 mm,1.8 μm),the mobile phase was 20 mmol/L ammonium acetate-0.1% formic acid aqueous solution,and the samples were sampled for 10 min and analyzed by mass spectrometry.Results The linear range of the three kinds of aconitine was 0.2-600 μg/L,and the correlation coefficient was greater than 0.998.The detection limits of the three kinds of aconitine were 0.10,0.20 and 0.20 μg/L,respectively.The recovery of the three kinds of aconitine were in the range of 66.0%-95.0%,and the relative standard deviations were in the range of 1.0%-5.0%.Conclusion The method is accurate,sensitive and selective.It is suitable for the determination of aconitum alkaloids and the diagnosis and analysis of food poisoning caused by aconitum alkaloids.