Determination of Scutellarin in Rabbit Plasma after Oral Administration by HPLC-MS with Solid-Phase Extraction  

固相萃取前处理HPLC-MS法测定口服给药后家兔血浆中的灯盏乙素(英文)

作　　者：李妮[1] 黄建明[1] 翁伟宇[1] 黄照昌[2] 蔡佳[1] 郁韵秋[1] 

机构地区：[1]复旦大学药学院,上海200032 [2]昆明制药集团股份有限公司,云南昆明650100

出　　处：《Journal of Chinese Pharmaceutical Sciences》2005年第1期38-42,共5页中国药学（英文版）

摘　　要：Aim To establish a sensitive and specific liquid chromatography-massspeetrometry 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-phaseextraction (SPE) was performed by using a Phenomenex C_8 cartridge. HPLC was carried out using aZorbax Extend-C_(18) column (150 mm x 2.1 mm ID, 5 μm) with a guard cartridge (Phenomenex) .Gradient elution was selected with the mobile phase of methanol 10 mmol·L^(-1) ammonium acetatesolution (pH adjusted to 8.0 with ammonia solution). The flow rate of mobile phase was 0.4mL·min^(-1) and the column temperature was 35 ℃ . Both scutellarin and the internal standard rutinin rabbit plasma extracts were detected by mass spectrometry using an ESI interface in the negativeion mode. Results The linear range was from 2 to 200 ng· mL^(-1), with acceptable accuracy andprecision (RSD) . Conclusion A sensitive, reliable and accurate method for the quantitation ofscutellarin in rabbit plasma has been established.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。

关 键 词：SCUTELLARIN LC-MS SPE BREVISCAPINE 

分 类 号：R285[医药卫生—中药学]