摘要
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(4.6mm×100mm,5μm)色谱分析枉,以98%CH3OH为流动相,流速0.3mL·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0.0125~2.0mg·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0.0125mg·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。
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% o 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.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2008年第1期55-57,共3页
Chinese Pharmaceutical Journal