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基于基质固相分散萃取结合二极管阵列与质谱检测的高效液相色谱法测定与鉴定黄芪中的异黄酮类成分

Determination and identification of isoflavonoids in Radix astragali by matrix solid-phase dispersion extraction and high-performance liquid chromatography with photodiode array and mass spectrometric detection.

作者信息

Xiao H B, Krucker M, Albert K, Liang X M

机构信息

Institute of Organic Chemistry, University of Tübingen, Auf der Morgenstelle 18, 72076 Tübingen, Germany.

出版信息

J Chromatogr A. 2004 Apr 2;1032(1-2):117-24. doi: 10.1016/j.chroma.2003.09.032.

Abstract

The isoflavonoids in Radix astragali were determined and identified by HPLC-photodiode array detection-MS after extraction employing matrix solid-phase dispersion (MSPD). As a new sample preparation method for R. astragali, the MSPD procedure was optimized, validated and compared with conventional methods including ultrasonic and Soxhlet extraction. The amounts of two major components in this herb, formononetin (6) and ononin (2), were determined based on their authentic standards. Four major isoflavonoids, formononetin (6), ononin (2), calycosin (5) and its glycoside (1), and three minor isoflavonoids, (6aR,11aR)-3-hydroxy-9, 10-dimethoxypterocarpan (7), its glycoside (3), and (3R)-7,2'-dihydroxy-3',4'-dimethoxyisoflavone-7-O-beta-D-glycoside (4), were identified based on their characteristic two-band UV spectra and [M + H], [aglycone + H]+ and [A1 + H]+ ions, etc. The combined MSPD and HPLC-DAD-MS method was suitable for quantitative and qualitative determination of the isoflavonoids in R. astragali.

摘要

采用基质固相分散(MSPD)萃取后,通过高效液相色谱-光电二极管阵列检测-质谱法对黄芪中的异黄酮进行了测定和鉴定。作为黄芪的一种新的样品制备方法,对MSPD程序进行了优化、验证,并与包括超声提取和索氏提取在内的传统方法进行了比较。基于其标准品测定了该药材中两种主要成分芒柄花素(6)和鹰嘴豆芽素A(2)的含量。根据四种主要异黄酮芒柄花素(6)、鹰嘴豆芽素A(2)、毛蕊异黄酮(5)及其糖苷(1)以及三种次要异黄酮(6aR,11aR)-3-羟基-9,10-二甲氧基紫檀烷(7)及其糖苷(3)和(3R)-7,2'-二羟基-3',4'-二甲氧基异黄酮-7-O-β-D-糖苷(4)的特征双波段紫外光谱以及[M + H]、[苷元 + H]+和[A1 + H]+离子等对其进行了鉴定。MSPD与HPLC-DAD-MS联用方法适用于黄芪中异黄酮的定量和定性测定。

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