氢核磁共振法测定中药茜草中大叶茜草素和羟基茜草素的含量

doi:10.3976/j.issn.1002-4026.2017.01.001

山东科学 ›› 2017, Vol. 30 ›› Issue (1): 1-7.doi: 10.3976/j.issn.1002-4026.2017.01.001

• 中药与天然活性产物 • 下一篇

氢核磁共振法测定中药茜草中大叶茜草素和羟基茜草素的含量

王志伟，闫慧娇，王晓，陈跃，林云良^*

山东省分析测试中心，山东省中药质量控制技术重点实验室，山东济南250014

收稿日期:2016-05-09 出版日期:2017-02-20 发布日期:2017-02-20
通信作者: 林云良。 Tel：0531-82605343；E-mail：wodekafei@126.com E-mail:wodekafei@126.com
作者简介:王志伟（1983—），男，博士，研究方向为中药效物质基础及质量控制，Email：wzwcpu@163.com
基金资助:
山东省科学院青年科学基金(2014QN005)；山东省自然科学基金三院联合基金(ZR2015YL012)

Quantitative determination of mollugin and purpurin from traditional Chinese medicine Rubiae Radix et Rhizoma by ¹H NMR

WANG Zhi-Wei, YAN Hui-Jiao, WANG Xiao, CHEN Yue, LIN Yun-Liang*

Shandong Provincial Key Laboratory for TCM Quality Control Technology, Shandong Analysis and Test Center, Shandong Academy of Sciences, Jinan, 250014

Received:2016-05-09 Online:2017-02-20 Published:2017-02-20

摘要/Abstract

摘要：

综合运用一维和二维核磁共振波谱技术，对茜草提取物中大叶茜草素、羟基茜草素的信号进行指认归属，并建立氢核磁共振法同时测定茜草中大叶茜草素、羟基茜草素含量的方法。在综合考虑茜草提取物的信号分离度及溶解性的基础上，最终选定氘代二甲基亚砜为测试溶剂，以大叶茜草素的烯烃信号(δ_H 5.77, H-2′)和羟基茜草素的H-3信号(δ_H 6.67)为定量峰，以顺丁烯二酸为定量内标。该方法具有较好的稳定性、重复性、精密度和准确性，且测定结果与HPLC-UV方法所得数据基本一致。所建立的氢核磁定量方法操作简单，测试时间短，且定量过程中不需要对照品，可用于中药茜草的质量控制及评价。

关键词: 大叶茜草素, 质量控制, 茜草, 羟基茜草素, 定量氢核磁共振

Abstract:

The ¹H chemical-shift values of mollugin and purpurin in extract from Rubiae Radix et Rhizoma were assigned on the basis of 1D and 2D NMR, and a specific, simple, sensitive 1H NMR method has been developed and validated for the simultaneous quantitative determination of mollugin in extract from Rubiae Radix et Rhizoma When the solvent effects on the resolution of target signals and the solubility of the crude extracts were taken into account, dimethyl sulfoxide-d₆ was selected as an optimal ¹H NMR solvent. Quantitative determination was carried out by using the signal of the olefinic proton of mollugin (δ_H 5.77, H-2′) and H-3 of purpurin (δ_H 6.67), which were not interfere with other signals. Maleic acid was selected as internal standard because of its stable physical and chemical properties and having simple resonance signal. The improved method possessed good stability, repeatability, precision and accuracy for the quantification of mollugin and purpurin and the determination results agreed with the data obtained by HPLC-UV method. Due to its simple operation, short test time and without any reference

中图分类号:

R284.1

王志伟，闫慧娇，王晓，陈跃，林云良. 氢核磁共振法测定中药茜草中大叶茜草素和羟基茜草素的含量[J]. 山东科学, 2017, 30(1): 1-7.

WANG Zhi-Wei, YAN Hui-Jiao, WANG Xiao, CHEN Yue, LIN Yun-Liang. Quantitative determination of mollugin and purpurin from traditional Chinese medicine Rubiae Radix et Rhizoma by ¹H NMR[J]. SHANDONG SCIENCE, 2017, 30(1): 1-7.

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氢核磁共振法测定中药茜草中大叶茜草素和羟基茜草素的含量

Quantitative determination of mollugin and purpurin from traditional Chinese medicine Rubiae Radix et Rhizoma by ¹H NMR

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氢核磁共振法测定中药茜草中大叶茜草素和羟基茜草素的含量

Quantitative determination of mollugin and purpurin from traditional Chinese medicine Rubiae Radix et Rhizoma by 1H NMR

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Quantitative determination of mollugin and purpurin from traditional Chinese medicine Rubiae Radix et Rhizoma by ¹H NMR