摘要
目的建立HPLC—MS／APCI测定SD大鼠血浆中齐墩果酸质量浓度的方法。方法色谱柱为Thermo BDS Hypersil C18（4．6mm×150mm，5μm）。流动相为甲醇-水（含1％。甲酸），梯度洗脱，流速1．0mL·min^-1，柱温40℃，地塞米松为内标，APCI源选择正离子监测，齐墩果酸m／z439．1，地塞米松（内标）m／z374．0．样品处理采用100μL血异丙醇及4mL氯仿液液萃取，有机层于50℃下氮气吹干，100μL甲醇定容，HPLC进样量为5μL.结果测定齐墩果酸的线性范围为0．063～2．500mg·L^-1，最低检测限为0．016mg·L^-1，日内精密度RSD〈9．38％，日间精密度RSI）〈8．96％。方法回收率范围为97．00％～99．69％.结论本方法精密、准确，适用于齐墩果酸在大鼠体内的药动学研究.
OBJECTIVE To constitute a HPLC-MS method for determining the concentration of oleanolic acid in rat plasma. METHODS Using Thermo BDS Hypersil C18（4.6 mm× 150 mm, 5 μm） columnn, the mobile phase consisted of methanol-water（ 1‰ formic acid） with step-gradient elution, the flow rate was 1.0 mL · min^-1, the column temperature was 40 ℃, the internal standard was dexamethasone. The compounds were ionized in the atmosphere pressure chemical ion （APCI） source of the mass spectrometer and were detected in theselected ionmonitoring （SIM） mode. The plasma samples were extracted by 100 μL isopropy and 4 mL chloroform, then the organic layer was evaporated to dryness at 50 ℃ by nitrogen. The residue was reconstituted by 100 μL methanol, and 5 μL was injected into the HPLC. RESULTS The linear range of oleanolic acid was 0. 063 - 2. 500 mg· L^- 1. The limit of detection was 0.016 mg· L^- 1. The within-day RSI） was below 9.38 % and between-day RSD was below 8.96%. Method recovery was between 97.00% to 99.69%. CONCLUSION The method is accuracy and sensitive for the pharmacokinetics of oleanolic acid in rats.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2006年第16期1265-1267,共3页
Chinese Pharmaceutical Journal
