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目的:建立UPLC/Q Exactive MS快速检测家兔血浆中乌头碱、次乌头碱和新乌头碱的方法。方法:采用Ulti Mate 3000系列高效液相色谱仪和Q Exactive四极杆-静电场轨道阱高分辨质谱系统检测。家兔血浆用2%甘油甲醇溶液沉淀蛋白后,以甲醇-水(0.2%甲酸,0.015%三乙胺)(80∶20)为流动相,DIONEX-C18色谱柱分离,通过高分辨质谱的全扫描/选择离子监测(Full MS/SIM)模式进行定性筛查和定量检测,以利血平为内标进行内标法定量。结果:乌头碱、次乌头碱、新乌头碱3种物质的线性关系良好,定量下限为0.02 ng/m L;血浆的萃取回收率及方法回收率高,分别在84.39%~89.14%、91.14%~99.12%范围内;3种成分的日内、日间精密度RSD均小于6.43%。结论:该方法适用于急性草乌中毒患者的血药浓度监控研究。
Objective: To establish a rapid UPLC / Q Exactive MS method for the detection of aconitine, hypaconitine and mesaconitine in rabbit plasma. Methods: Ulti Mate 3000 series HPLC and Q Exactive quadrupole - electrostatic field orbitrap high resolution mass spectrometry were used. After the rabbit plasma was precipitated with 2% glycerol methanol, the mobile phase was separated on a DIONEX-C18 column with methanol-water (0.2% formic acid, 0.015% triethylamine) Scanning / selective ion monitoring (Full MS / SIM) mode for qualitative screening and quantitative detection, reserpine standard internal standard quantification. Results: There was a good linear relationship between aconitine, hypaconitine and mesaconitine. The lower limit of quantification was 0.02 ng / m L. The recovery rate of plasma and its recovery was high from 84.39% to 89.14% , 91.14% ~ 99.12%. The RSDs of intra-day and inter-day precision of the three components were less than 6.43%. Conclusion: This method is suitable for the monitoring of blood concentration in patients with acute grass poisoning.