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一种用于评估达玛烷型人参皂苷纯度的通用定量¹H核磁共振(qNMR)方法。

A universal quantitative ¹H nuclear magnetic resonance (qNMR) method for assessing the purity of dammarane-type ginsenosides.

作者信息

Li Ze Yun, Welbeck Edward, Wang Ru Feng, Liu Qing, Yang Ying Bo, Chou Gui Xin, Bi Kai Shun, Wang Zheng Tao

机构信息

School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, 110016, China.

出版信息

Phytochem Anal. 2015 Jan-Feb;26(1):8-14. doi: 10.1002/pca.2527. Epub 2014 Jun 9.

DOI:10.1002/pca.2527
PMID:24912845
Abstract

INTRODUCTION

Quantitative (1)H-NMR (qNMR) is a well-established method for quantitative analysis and purity tests. Applications have been reported in many areas, such as natural products, foods and beverages, metabolites, pharmaceuticals and agriculture. The characteristics of quantitative estimation without relying on special target reference substances make qNMR especially suitable for purity tests of chemical compounds and natural products. Ginsenosides are a special group of natural products drawing broad attention, and are considered to be the main bioactive principles behind the claims of ginsengs efficacy. The purity of ginsenosides is usually determined by conventional chromatographic methods, although these may not be ideal due to the response of detectors to discriminate between analytes and impurities and the long run times involved.

OBJECTIVE

To establish a qNMR method for purity tests of six dammarane-type ginsenoside standards.

METHODS

Several experimental parameters were optimised for the quantification, including relaxation delay (D1), the transmitter frequency offset (O1P) and power level for pre-saturation (PL9). The method was validated and the purity of the six ginsenoside standards was tested. Also, the results of the qNMR method were further validated by comparison with those of high performance liquid chromatography.

CONCLUSION

The qNMR method was rapid, specific and accurate, thus providing a practical and reliable protocol for the purity analysis of ginsenoside standards.

摘要

引言

定量氢核磁共振(qNMR)是一种成熟的定量分析和纯度检测方法。其应用已在许多领域有所报道,如天然产物、食品和饮料、代谢物、药物及农业领域。qNMR不依赖特殊目标参考物质进行定量估计的特点,使其特别适用于化合物和天然产物的纯度检测。人参皂苷是一类备受广泛关注的特殊天然产物,被认为是人参功效宣称背后的主要生物活性成分。人参皂苷的纯度通常通过传统色谱方法测定,不过由于检测器区分分析物和杂质的响应以及所需的较长运行时间,这些方法可能并不理想。

目的

建立一种用于六种达玛烷型人参皂苷标准品纯度检测的qNMR方法。

方法

对定量的几个实验参数进行了优化,包括弛豫延迟(D1)、发射机频率偏移(O1P)和预饱和功率水平(PL9)。对该方法进行了验证,并检测了六种人参皂苷标准品的纯度。此外,通过与高效液相色谱法的结果进行比较,进一步验证了qNMR方法的结果。

结论

qNMR方法快速、特异且准确,从而为参皂苷标准品的纯度分析提供了一种实用且可靠的方案。

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