UPLC—MS／MS法测定人血中雪上一枝蒿甲素

目的建立超高效液相色谱-串联质谱（UPLC—MS／MS）法测定人血中雪上一枝蒿甲素含量的方法。方法样品经乙酸乙酯提取后，Ci8柱分离，以0．1％甲酸乙腈-0．1％甲酸水为流动相梯度洗脱，正离子-多反应离子监测模式（ESI＋-MRM）测定雪上一枝蒿甲素，定性定量离子对分别为344．3／58．0、344．3／91．0。结果雪上一枝蒿甲素在3．5～850ug／L-1。范围内与峰面积呈现良好的线性关系（r=-0．9968），检测限为0．1Iμg／L-1，日内、日间精密度均〈10％，低、中、高三个浓度下准确度（n=5）为97．2％-115．2％，回收率（n=5）为86．6％~89．4％。结论该方法操作简便，结果准确，可作为测定人血中雪上一枝蒿甲素含量的方法。

Determination of Bullatine A in Human Blood by UPLC-MS/MS

Objective To determine bullatine A in human blood by UPLC-MS/MS. Methods The sample was extracted with acetic ether and separated on a Cls column using, 0.1% formic acid and acetonitrile as mobile phase. The positive electrospray ionization source was used. The ion pairs for the anaylsis of bullatine A were 344.3/58.0 and 344.3/91.0 in the multiple reaction monitoring mode. Results Linear relationship between peak area and concentration of bullatine A was obtained in the range of 3.5-850 μg/L-1 @=0.9968）. The limit of detection for the analyte was 0.1μg/L-L Relative standard deviations （RSD） （n=6） for the intra-day and inter-day precisions were lower than 10%. At three spiked concentrations, accuracy （n=5） ranged from 97.2% to 115.2%, and recovery ranged from 86.6% to 89.4%. Matrix effect was not obvious. Conclusion The established method is simple, sensitive, and accurate. It can be used for the determination of bullatine A in human blood.