大鼠灌服枳实提取液后体内黄酮类代谢产物的LC-MS/MS分析  

Identification of flavonoid metabolites of Fructus Aurantii Immaturus in rat biological samples by liquid chromatography-tandem mass spectrometry

作　　者：李哲[1,2] 宋瑞[1,2] 许风国[1,2] 许磊[1,2] 田媛[1,2] 张尊建[1,2] 

机构地区：[1]药物质量与安全预警教育部重点实验室 [2]中国药科大学分析测试中心,南京210009

出　　处：《中国药科大学学报》2010年第6期539-547,共9页Journal of China Pharmaceutical University

基　　金：国家自然科学基金资助项目(No.30672587)~~

摘　　要：建立了高效液相色谱-串联质谱分析方法,分析大鼠灌服枳实提取液后尿液、粪便和胆汁中的黄酮类成分。采用色谱柱为Agilent Zorbax SB-C18柱(250mm×4.6mm,5μm);流动相为0.1%甲酸水溶液-甲醇-乙腈三元梯度洗脱系统,柱温35℃,流速1.0mL/min;采用电喷雾离子化源-三重四极杆质谱系统,负离子模式检测。在枳实提取液中共检出了34种黄酮类成分,在大鼠生物样本中共检出40种黄酮类成分,其中14种来源于体外,26种为代谢产物,并初步归属了它们的结构。High-performance liquid chromatography with tandem mass spectrometry（HPLC-MS/MS） was used for separation and identification of flavonoid metabolites in rat urine,feces and bile after oral administration of the Citrus sinensis extraction.The HPLC experiments used a reversed-phase Zorbax SB-C18 column with the column temperature of 35 °C and a binary mobile phase system consisting of aqueous formic acid（0.1%） and methanol-acetonitrile（3：2） using a gradient elution with the flow rate of 1.0 mL/min.The ESI-MS/MS was operated with a triple-quadruple mass spectrometer in negative ion mode.A total of 34 flavonoid compounds in vitro and 40 flavonoid compounds including 14 parent compounds and 26 metabolites in vivo were detected,and they were tentatively identified.The identification of these metabolites provided essential data for further pharmacological and clinical studies of Citrus sinensis Osbeck.and related preparations.

关 键 词：枳实 黄酮 代谢产物 体内代谢 高效液相谱-串联质谱法 

分 类 号：R285.5[医药卫生—中药学]