HPLC-MS-MS测定人尿液中黄芪甲苷浓度及其尿液药动学研究

 目的建立HPLC-MS-MS测定人尿液中黄芪甲苷的浓度。方法使用C₁₈(4.6 mm×100 mm,5μm)色谱分析柱,以98%CH₃OH为流动相,流速0.3 mL·min^-1。尿液样品经甲醇沉淀后进样,选择黄芪甲苷离子对(807.3/627.3m/z)为选择性检测离子,按外标法定量。结果尿液中黄芪甲苷线性范围为0.012 5～2.0 mg·L^-1,日内和日间RSD均小于6%,方法回收率在97.5%～104.2%,最低定量质量浓度为0.012 5 mg·L^-1。结论本方法简便、快速、特异,适用于黄芪甲苷人体药动学研究。

Determination of Astragaloside IV in Human Urine by a HPLC-MS-MS Method

OBJECTIVE To establish a sensitive and specific HPLC-MS-MS method for the determination of Astragaloside Ⅳ in human urine.METHODS The Kromasil C₁₈(4.6 mm×100 mm,5 μm)analytic column was used.98% Methanol was used as mobile phase at the flow rate of 0.3 mL·min^-1.Detection was performed on API mass spectrometry equipped with an ESI and operated in positive-ionization mode.Astragaloside quantitation in urine was calculated by computing the peak area of Astragaloside Ⅳ(807.3/627.3).RESULTS The calibration curve was linear over the range of 0.012 5～2.0 mg·L^-1 in human urine,and the within-day and between-day precisions were less than 6%.The method recovery was 97.5%～104.2%.CONCLUSION HPLC-MS-MS Method established in this study is simple,sensitive with precision,which can be adapted to pharmacokinetic study.