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用 HPLC-DAD 和 HPLC-ESI-MS 分析水飞蓟宾制剂的成分。

Analysis of the constituents of aqueous preparations of Stachys recta by HPLC-DAD and HPLC-ESI-MS.

机构信息

Department of Pharmaceutical Sciences, University of Florence, Via Ugo Schiff 6, 50019, Sesto Fiorentino (FI), Firenze, Italy.

出版信息

J Pharm Biomed Anal. 2010 Sep 21;53(1):15-23. doi: 10.1016/j.jpba.2010.03.002. Epub 2010 Mar 7.

Abstract

In the present study a method based on liquid chromatography with diode array detection (HPLC/DAD) coupled to an electrospray ionization (ESI) interface for the simultaneous determination of phenolic constituents in three aqueous preparations of the herbal medicinal drug Stachys recta. The developed assay was simple and effective and permitted the quality control of S. recta decoctions and infusion. Overall, 30 constituents were detected and identified, belonging mainly to three classes of compounds: caffeoylquinic acids, phenylethanol glycosides and flavonoids. 15 of them were quantified having a lower limit not less than 0.02% of the lyophilized extracts. Only seven of them were previously reported in this species, while 23 were identified for the first time as constituents of S. recta. HPLC-DAD-ESI-MS analysis provided evidence for the certain identification of the main constituents and in some cases of their isomers. Eight constituents were isolated and their structure elucidated by HPLC-ESI-MS and 1D- and 2D-NMR spectroscopy. Among the investigated preparations, the infusion seems to be the best method to extract the native constituents of the plant, while decoction is a more aggressive treatment and causes partial degradation of some acylated flavonoids.

摘要

本研究建立了一种基于高效液相色谱二极管阵列检测(HPLC/DAD)与电喷雾电离(ESI)接口联用的方法,用于同时测定三种水提草药水苏的酚类成分。所建立的方法简单有效,可用于水苏汤和水苏浸剂的质量控制。该方法共检测并鉴定了 30 种成分,主要属于 3 类化合物:咖啡酰奎宁酸、苯乙醇苷和黄酮类。其中 15 种成分定量检测限不低于干浸膏的 0.02%。其中有 7 种为该种植物中首次报道的成分,23 种为水苏中的首次鉴定成分。HPLC-DAD-ESI-MS 分析为主要成分的鉴定提供了证据,在某些情况下还为其同分异构体的鉴定提供了证据。对 8 种成分进行了分离,并通过 HPLC-ESI-MS 和 1D 和 2D-NMR 光谱对其结构进行了鉴定。在所研究的制剂中,浸剂似乎是提取植物天然成分的最佳方法,而汤剂则是一种更具侵略性的处理方法,会导致一些酰化黄酮类化合物部分降解。

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