Hunan University of Chinese Medicine, School of Pharmacy, Academician Atta-ur-Rahman Belt and Road Traditional Medicine Research Center, TCM and Ethnomedicine Innovation & Development International Laboratory, Changsha, Hunan, P. R. China, 4108208.
Tasly Holding Group Co., Ltd, Tasly Academy, Tianjin, P. R. China, 300410.
J AOAC Int. 2021 May 21;104(2):506-514. doi: 10.1093/jaoacint/qsaa130.
Qishen Yiqi dripping pills (QSYQ), composed of four herbal medicines-Salvia miltiorrhiza, Astragalus membranaceus, Panax notoginseng, and Dalbergiaodorifera-are widely used to treat ischemic cerebrovascular and hemorrhagic cerebrovascular conditions.
In this study, a rapid and accurate proton NMR (1HNMR) spectroscopy method was established to control the quality of QSYQ and ensure their clinical efficacy.
Firstly, different types of metabolites were identified based on the proton signal peaks of chemical shifts, coupling constants, and related information provided through two-dimensional NMR spectroscopy. Secondly, a quantitative 1HNMR method was established for the simultaneous determination of major constituents in QSYQ samples. In addition, an HPLC method was performed to verify the results obtained by the quantitative proton NMR (qHNMR) method.
In the present study, 26 metabolites were identified in the 1HNMR spectra of QSYQ. In addition, a rapid and accruate qHNMR method was established for the simultaneous determination of protocatechualdehyde, rosmarinic acid, danshensu, calycosin-7-O-β-D-glucoside, and ononin in ten batches of QSYQ samples for the first time. Moreover, the proposed qHNMR method and HPLC method were compared using Bland-Altman and plots Passing-Bablok regression, indicating no significant differences and a strong correlation between the two analytical methods.
This method is an important tool for the identification and quantification of major constituents in QSYQ.
Compared with traditional HPLC, the established qHNMR method has the advantages of simple sample preparation, short analysis time, and non-destructive analysis.
芪参益气滴丸由丹参、黄芪、三七、降香 4 味中药组成，广泛用于治疗缺血性和出血性脑血管病。
本研究建立了一种快速准确的质子核磁共振（1HNMR）光谱法，用于控制 QSYQ 的质量，确保其临床疗效。
首先，根据化学位移、偶合常数和二维 NMR 光谱提供的相关信息，基于质子信号峰鉴定不同类型的代谢物。其次，建立了一种用于同时测定 QSYQ 样品中主要成分的定量 1HNMR 方法。此外，还进行了高效液相色谱法（HPLC）验证。
在本研究中，在 QSYQ 的 1HNMR 图谱中鉴定出 26 种代谢物。此外，首次建立了一种快速准确的定量质子 NMR（qHNMR）方法，用于同时测定 10 批 QSYQ 样品中的原儿茶醛、迷迭香酸、丹参素、毛蕊异黄酮-7-O-β-D-葡萄糖苷和芒柄花苷。而且，通过 Bland-Altman 和 Passing-Bablok 回归图比较了所提出的 qHNMR 方法和 HPLC 方法，表明两种分析方法之间没有显著差异，具有很强的相关性。
该方法是鉴定和定量 QSYQ 中主要成分的重要工具。
与传统的 HPLC 相比，所建立的 qHNMR 方法具有样品制备简单、分析时间短、无损分析等优点。
