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目的:建立测定血浆中雷公藤红素药物浓度的UPLC-MS/MS方法,测定健康受试者和HIV患者血浆中该药药物浓度及研究其药动学。方法:以伪人参皂苷代谢产物DQ为内标物,血浆样本采用乙酸乙酯液液萃取法处理,流动相为甲醇/0.3%甲酸-水溶液;用ACQUITY UPLC BEH C18(2.1mm×50mm,1.7μm)色谱柱梯度洗脱。质谱检测采用ESI离子源,正离子模式,MRM检测模式,用于定量的离子反应为m/z 451.2→m/z 201.3(雷公藤红素)和为m/z 477.2→m/z 143.2(DQ)。1名健康受试者单剂量口服雷公藤多苷片20mg,19例免疫无应答HIV患者多剂量口服雷公藤多苷片10mg或20mg后,采集血浆样本进行测定。结果:雷公藤红素在(0.05-25.0)ng/m L,线性关系良好;最低定量限为0.05ng/m L;质控样本(0.25、2.50、20.0ng/m L)批内精密度和批间精密度RSD均<15%,提取回收率>80%。健康受试者雷公藤红素血浆药物浓度最高为0.52ng/m L,HIV患者血浆药物浓度为0.28-4.01ng/m L。结论:本研究所建立的UPLC-MS/MS方法灵敏、准确、可靠,可用于人血浆中雷公藤红素药物浓度的测定及药动学研究。
OBJECTIVE: To establish an UPLC-MS / MS method for the determination of barbiturates in plasma and to determine the concentration of the drug in plasma of healthy subjects and HIV patients and to study its pharmacokinetics. Methods: The pseudo-ginsenoside metabolite DQ was used as the internal standard. The plasma samples were treated with ethyl acetate liquid-liquid extraction and the mobile phase consisted of methanol / 0.3% formic acid-water. The cells were eluted with ACQUITY UPLC BEH C18 (2.1 mm × 50 mm, 1.7 μm ) Column gradient elution. Mass spectrometry was performed with ESI ion source, positive ion mode, and MRM detection mode and the ion reaction for quantification was m / z 451.2 → m / z 201.3 (tripterine) and m / z 477.2 → m / z 143.2 (DQ ). A healthy volunteer oral single dose of tripterygium glycosides tablets 20mg, 19 cases of immunocompromised HIV multi-dose oral administration of Tripterygium tablets 10mg or 20mg, plasma samples were collected for determination. Results: Tripterine had a good linear relationship (0.05-25.0 ng / m L), the lowest limit of quantification was 0.05 ng / m L, the intrabatch precision of control samples (0.25, 2.50 and 20.0 ng / m L) Inter-batch precision RSD <15%, extraction recovery> 80%. The highest plasma concentration of tripterine in healthy subjects was 0.52 ng / m L, and the plasma drug concentration in HIV patients was 0.28-4.01 ng / m L. Conclusion: The UPLC-MS / MS method established in this study is sensitive, accurate and reliable and can be used for the determination and pharmacokinetic study of tripterine in human plasma.