【摘要】 目的　建立灵敏、专属的HPLC ESI MS测定法 ,用于测定家兔口服灯盏花素缓释片 (2片 6 0mg/片 )后的血药浓度。方法　该定量方法采用芦丁作内标 ,用固相萃取 (SPE)进行样品前处理。以甲醇 10mmol·L-1醋酸铵水溶液 (pH 8 .0 )梯度洗脱 ,流动相流速 0 .4mL·min-1,柱温 35℃ ,经过Zorbax Extend C18(15 0mm× 2 . 1mmID ,5 μm)色谱柱分离 ,电喷雾质谱检测器在负离子模式下检测灯盏乙素和芦丁。结果　在 2～ 2 0 0ng·mL-1范围内灯盏乙素与内标峰面积与浓度线性关系良好 ,且准确度、精密度满足生物样品分析的要求。结论　本实验建立的兔血浆中灯盏乙素的HPLC MS分析方法灵敏度高 ,可用于口服给药后灯盏乙素的血药浓度测定。更多还原

【Abstract】 Aim To establish a sensitive and specific liquid chromatography-mass s pectrometry method for determination of scutellarin in rabbit plasma after oral administration. Methods For the quantitative analysis, rutin was used as an internal standard and solid-phase extraction (SPE) was performe d by using a Phenomenex C 8 cartridge. HPLC was carried out using a Zorbax Exte nd-C 18column (150 mm×2.1 mm ID, 5 μm) with a guard cartridge (Phenome n ex). Gradient elution was selected with the mobile phase of methanol 10 mmol·L -1 ammonium acetate solution (pH adjusted to 8.0 with ammonia soluti on). The flow rate of mobile phase was 0.4 mL·min -1 and the column temperatur e was 35 ℃. Both scutellarin a nd the internal standard rutin in rabbit plasma extracts were detected by mass s pectrometry using an ESI interface in the negative ion mode. Results The linear range was from 2 to 200 ng·mL -1, with acceptable accuracy and precision (RSD). Conclusion A sensitive, reliable and accurate method for the quantitati on of scutellarin in rabbit plasma has been established.更多还原