液质联用分析葛根提取物及中药片剂中异黄酮类化合物  

Separation and Identification of Isoflavonoids in Pueraria lobata Extracts and Its Preparations by Reversed-Phase Capillary Liquid Chromatography Coupled with Electrospray Ionization Quadrupole Time of Flight Mass Spectrometry

作　　者：田宏哲[1] 王华[1] 关亚风[1] 

机构地区：[1]中国科学院大连化学物理研究所,辽宁大连116023

出　　处：《色谱》2005年第5期477-481,共5页Chinese Journal of Chromatography

基　　金：国家自然科学基金仪器专项基金资助项目(批准号20227501);中国科学院大型科学仪器装备支持计划项目;大连化学物理研究所科学创新项目

摘　　要：采用反相C18毛细管液相色谱柱,以乙腈(含0.1%(体积分数,下同)三氟乙酸)和水(含0.1%三氟乙酸)为流动相梯度洗脱,在26 min内分离了葛根异黄酮提取物以及愈风宁心片中的主要成分.采用毛细管液相色谱/四极杆飞行时间串联质谱仪对葛根提取物以及片剂中的几种主要异黄酮类化合物做了结构分析,发现葛根素是主成分(提取物中其平均质量分数是13.32% ;片剂中每片含量19.28～24.34 mg).对微量未知化合物,用它们的子离子谱图与已知化合物的谱图比较,推测其成分为3'-甲氧基葛根素和3'-甲氧基大豆苷.Isoflavonoids in Pueraria lobata extract and its preparations were separated and identified by reversed-phase capillary liquid chromatography （RP-CapLC） coupled with photodiode array （PDA） detector and negative electrospray ionization quadrupole time of flight （QTOF） mass spectrometry. The separation was performed on a 150 mm × 0. 32 mm i. d. , 5 μm C18 capillary column, using mobile phase of 0. 1% aqueous trifluoroacetic acid solution and acetonitrile containing 0. 1% trifluoroacetic acid under gradient elution. The product ion spectra of the deprotonated ions allowed for the identification of puerarin, daidzin and daidzein in the sample. Puerarin was found to be the most abundant component in the extract （about 13%, mass fraction） and its preparations （ 19.28 - 24. 34 mg per tablet）. The structures of trace amount of unknown isoflavonoids were deduced based on the spectra of known compounds. They were proposed to be 3＇-methoxypuerarin and 3＇-methoxydaidzin.

关 键 词：反相毛细管液相色谱 液相色谱-电喷雾离子质谱 葛根异黄酮 葛根素 中药 

分 类 号：O658[理学—分析化学]