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(1)H-NMR 定量分析的白芍中五种蒽醌成分的组成变化。

Developmental changes in the composition of five anthraquinones from Rheum palmatum as quantified by (1) H-NMR.

机构信息

State Key Laboratory of Natural Medicines, Department of Natural Medicinal Chemistry, China Pharmaceutical University, 24 Tong Jia Xiang, Nanjing 210009, People's Republic of China.

出版信息

Phytochem Anal. 2013 Jul-Aug;24(4):329-35. doi: 10.1002/pca.2414. Epub 2013 Jan 31.

Abstract

INTRODUCTION

Rheum palmatum is an important traditional Chinese medicine featuring anthraquinones with several activities. Generally, rhein, emodin, aloe-emodin, physcion and chrysophanol are used as chemical markers for the quality control of rhubarb products.

OBJECTIVE

To develop a simple protocol for the quantification of rhein, emodin, aloe-emodin, physcion and chrysophanol in R. palmatum collected at different developmental stages.

METHODS

(1) H-NMR spectra were measured on samples dissolved in acetone-d6 , quantification was carried out using the signals of H-4 of rhein (δH 8.36), H-7 of emodin (δH 6.68), CH2 OH of aloe-emodin (δH 4.81), OCH3 of physcion (δH 4.02) and CH3 of chrysophanol (δH 2.50), which were well separated from other signals. Quantitative analysis was based on the relative ratio of the intensity of each compound to the known amount of internal standard maleic acid.

RESULTS

The quantitative (1) H-NMR (qHNMR) method developed showed good precision, trueness, linearity, repeatability and stability for the quantification of rhein, emodin, aloe-emodin, physcion and chrysophanol. This method was applied successfully to explore the seasonal variations of the five major anthraquinones in R. palmatum, and provided quantitative results in reasonable agreement with those obtained by the HPLC-UV method.

CONCLUSION

Compared with the conventional HPLC-based methods, the qHNMR analysis is rapid, reference-free and convenient with less sample pre-treatment. This technique should be a feasible choice for the quality control of R. palmatum.

摘要

简介

大黄是一种重要的传统中药,其主要活性成分为蒽醌类化合物。一般来说,大黄酸、大黄素、芦荟大黄素、大黄素甲醚和大黄酚常被用作大黄药材及其制剂的质量控制指标。

目的

建立一种简单的方法,用于测定不同生长发育阶段掌叶大黄中大黄酸、大黄素、芦荟大黄素、大黄素甲醚和大黄酚的含量。

方法

(1)采用氘代丙酮溶解样品,通过大黄酸 H-4 信号(δH 8.36)、大黄素 H-7 信号(δH 6.68)、芦荟大黄素 CH2 OH 信号(δH 4.81)、大黄素甲醚 OCH3 信号(δH 4.02)和大黄酚 CH3 信号(δH 2.50)进行定量分析,这些信号均与其他信号完全分离。定量分析基于每个化合物的强度与已知量内标马来酸的相对比值。

结果

所建立的定量核磁共振(qHNMR)方法具有良好的精密度、准确度、线性、重复性和稳定性,可用于测定大黄酸、大黄素、芦荟大黄素、大黄素甲醚和大黄酚的含量。该方法成功应用于掌叶大黄中五种主要蒽醌类化合物的季节性变化研究,其定量结果与 HPLC-UV 方法具有良好的一致性。

结论

与传统的 HPLC 方法相比,qHNMR 分析快速、无需参考标准品且方便,样品预处理工作量较少。该技术应是掌叶大黄质量控制的可行选择。

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