UPLC-MS/MS法测定人血中雪上一枝蒿甲素

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

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,C_(18)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3.5~850μg/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0.1μg/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。

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.