摘要
Cynanchum paniculatum(Bunge) Kitagawa is usually used as an herbal medicine for treating many diseases. Paeonol is the main active component, and its content is the key indicator for quality control of C. paniculatum. In the present study, we developed a rapid, accurate and precise method for quantitation of paeonol in C. paniculatum using 1 H NMR spectra. The deuterated solvent of methanol-d4 enabled satisfactory separation of the signals to be integrated in 1 H NMR spectrum. H-6(δ 7.78) of 1 H NMR spectrum of C. paniculatum was selected as the feature signal for quantitation, and trimesic acid(TMA) was selected as an internal standard. Validation of the quantitative method was performed in terms of linearity, specificity, repeatability and stability. This is the first time to report quantitative 1 H NMR(qHNMR) applied to determine the content of paeonol in C. paniculatum and showed a wider linearity range than the reported quantitation of paeonol in others. The simple extraction of paeonol from C. paniculatum was rapid and will prompt the application of the developed method. This work implied that qHNMR represented a feasible alternative to HPLC-based methods for quantitation of paeonol in C. paniculatum, and it was suitable for the quality control of C. paniculatum.
徐长卿是一种治疗多种疾病的中药材。丹皮酚是徐长卿的主要活性成分,也是质量控制的关键指标物。本文以核磁共振氢谱建立了一种徐长卿中丹皮酚含量的快速、准确、精密的检测方法。结果表明,氘代甲醇作溶剂可以很好的实现核磁共振氢谱中信号的分离,H-6 (δ7.78)可用作定量分析特征信号,均苯三甲酸用作内标。所建立的方法经线性范围、专属性、重复性和稳定性进行了确证。本文首次采用定量核磁共振氢谱检测徐长卿中丹皮酚的含量,线性范围较其他药材中丹皮酚的含量检测更宽。采用单次提取方式对丹皮酚进行提取,方法快速,更利于应用于质量控制中。本文研究表明相对现有基于高效液相色谱检测方法,定量核磁共振氢谱法是一种适合徐长卿质量控制可行的替代方法。
基金
Science and Technology Project of Yunnan Provincial Department of Science and Technology(Grant No.2018FD081)
Yunnan Local Colleges Applied Basic Research Projects[Grant Nos.2019FH001-(109),2017FH001-092,2017FH001-094 and 2018FH001-019]
Youth Research Foundation of Qujing Normal University in 2019(Grant No.2019QN004)。