论文部分内容阅读
目的:建立人血浆中倍他米松17-丙酸酯(B17P)的LC-MS/MS测定方法,并研究其在健康人体内的药动学特征。方法:采用Agilent Zorbax C18(2.1 mm×100 mm,3.5μm)色谱柱,以甲醇-水(88:12)为流动相,流速0.15 ml·min~(-1);电喷雾(ESI)离子源,正离子电离模式,多反应离子监测(MRM)的扫描方式,B17P和二丙酸倍氯米松(内标,IS)的检测离子对分别选择为m/z 471.1→397.1和543.2→433.1。结果:B17P的线性范围为0.02～2.0 ng·ml~(-1)(r=0.999 3,n=5),定量下限为0.02 ng·ml~(-1),日内和日间精密度(RSD)均小于10.9%,提取回收率在70%左右,方法回收率均在94.5～106.6%范围内。B17P的t_(1/2)为(82.5±17.3)h,C_(max)为(0.73±0.18)h,AUC_(0～1)为(63.9±13.6)ng·h·ml~(-1)。结论:该法简便、快速、灵敏、准确,适用于B17P血药浓度测定及其人体药动学研究。
Objective: To establish a LC-MS / MS method for the determination of betamethasone 17-propionate (B17P) in human plasma and study its pharmacokinetics in healthy volunteers. METHODS: The mobile phase consisted of methanol and water (88:12) at a flow rate of 0.15 ml · min -1 on an Agilent Zorbax C18 (2.1 mm × 100 mm, 3.5 μm) column. Electrospray (ESI) , Positive ionization mode, multi-reactive ion monitoring (MRM) scanning mode, and the ion pairs of B17P and beclomethasone dipropionate (internal standard, IS) were selected as m / z 471.1 → 397.1 and 543.2 → 433.1, respectively. Results: The linear range of B17P was 0.02-2.0 ng · ml -1 (r = 0.999 3, n = 5). The lower limit of quantification was 0.02 ng · ml -1. The intra- and inter-day precision ) Were less than 10.9%, the recovery rate was about 70%, the recovery rates were 94.5 ~ 106.6%. The t 1/2 of B17P was (82.5 ± 17.3) h, the C max was 0.73 ± 0.18 h, and the AUC 0-1 was 63.9 ± 13.6 ng · h · ml -1 . Conclusion: The method is simple, rapid, sensitive and accurate and suitable for the determination of B17P and its pharmacokinetics.