论文部分内容阅读
目的建立快速检测人尿液和全血中乌头碱、新乌头碱和次乌头碱的超高压液相色谱-串联质谱分析方法。方法尿液样品直接进样,全血样品经乙腈-甲醇(9:1,v/v)沉淀蛋白,以甲醇和5.0 mmol/L碳酸氢铵水溶液作为流动相进行梯度洗脱,在BEH C18色谱柱上实现分离,电喷雾正离子多反应监测方式检测,以那可丁作为内标的基质标准内标法定量。结果尿液和全血中3种乌头生物碱的平均加标回收率分别为93.9%～108%和89.7%～109%,相对标准偏差为1.3%～11%和1.1%～18%(n=6),定量限(S/N=10)分别为0.05μg/L和0.1μg/L。结论此方法灵敏、准确,已成功应用于一起中毒事件的检测。
OBJECTIVE To establish a method for the rapid determination of aconitine, mesaconitine and hypaconitine in human urine and whole blood by ultra-high performance liquid chromatography-tandem mass spectrometry. Methods Urine samples were directly injected. The whole blood samples were precipitated with acetonitrile-methanol (9: 1, v / v) and eluted with methanol and 5.0 mmol / L aqueous ammonium bicarbonate solution as mobile phase. Column separation, electrospray positive ion detection of multi-reaction monitoring method, with Nadine as the internal standard matrix standard internal standard method. Results The average recoveries of three aconitine alkaloids in urine and whole blood were 93.9% -108% and 89.7% -109%, respectively, and the relative standard deviations were 1.3% ~ 11% and 1.1% ~ 18% (n = 6). The limits of quantitation (S / N = 10) were 0.05 μg / L and 0.1 μg / L, respectively. Conclusion This method is sensitive and accurate and has been successfully applied in the detection of poisoning events.