高效液相色谱-质谱联用法测定人血浆中非那雄胺的浓度

Determination of finasteride in human plasma by HPLC-MS

目的:建立一种用高效液相色谱电喷雾离子化质谱(HPLCMS)联用技术测定非那雄胺血药浓度的方法。方法:以0.01mol·L-1醋酸铵水溶液甲醇(25∶75)为流动相,烯酮二醇为内标。血浆样品经用醋酸乙酯萃取后上样,经C18柱分离后,以质谱为检测器,采用选择性离子检测(SIM)测定人体血浆中非那雄胺的浓度。结果:非那雄胺的线性范围0.491～98.2μg·L-1(r=0.9999),平均相对回收率在90%～110%之间,日内和日间RSD均<5%,非那雄胺的最低定量限为0.49μg·L-1,提取回收率>90%。结论:该方法快速、准确、灵敏,可用于非那雄胺的药动学研究。

OBJECTIVE To develop an high-performance liquid chromatography and electrospray ionization mass spectrometry（HPLC-ESI-MS） method for determination of finasteride in human plasma. METHODS The mobile phase was composed of 0. 01mol·L^1 ammonium acetate/water： methanol（25：75）. Plasma samples were extracted with ethyl acetate and separated by C18column.The single quadrapole MS was used as detector. Selected ion monitor （SIM） was used for determination of finasteride in human plasma. RESULTS Standard curve was linear in the range of 0. 491 - 98. 2μg·L^-1 （r = 0. 999 9）, the relative recovery was between 90%-110%. Relative standard deviation （RSD） of intra-day and inter-day assays were all less than 5%. The quantitation limit was0. 49μg·L^-1. The extraction recovery was more than 90%. CONCLUSION The method proves to be a stable and reliable method for determination of finasteride in human plasma as well as for pharmacokinetic studies.