采用二维 qNMR 法测定番泻叶、番泻果和片剂中的总番泻苷及番泻苷 A、B、A。
Determination of Total Sennosides and Sennosides A, B, and A in Senna Leaflets, Pods, and Tablets by Two-Dimensional qNMR.
机构信息
Pharmazeutisches Institut, Abteilung Pharmazeutische Biologie, Christian-Albrechts-Universität zu Kiel, Gutenbergstraße 76, 24118 Kiel, Germany.
Pharmazeutisches Institut, Abteilung Pharmazeutische und Medizinische Chemie, Christian-Albrechts-Universität zu Kiel, Gutenbergstraße 76, 24118 Kiel, Germany.
出版信息
Molecules. 2022 Oct 29;27(21):7349. doi: 10.3390/molecules27217349.
In the present work, a two-dimensional qNMR method for the determination of sennosides was established. Using band-selective HSQC and the cross correlations of the characteristic 10-10' bonds, we quantified the total amount of the value-determining dianthranoids in five minutes, thus, rendering the method not only fast, but also specific and stability indicating. The validation of the method revealed excellent accuracy (recovery rates of 98.5 to 103%), precision (RSD values of 3.1%), and repeatability (2.2%) and demonstrated the potential of 2D qNMR in the quality control of medicinal plants. In a second method, the use of 2D qNMR for the single analysis of sennosides A, B, and A was evaluated with acceptable measurement times (31 min), accuracy (93.8%), and repeatability (5.4% and 5.6%) for the two major purgatives sennoside A and B. However, the precision for sennoside B and A was not satisfactory, mainly due to the low resolution of the HSQC signals of the two compounds.
在本工作中，建立了一种用于测定番泻苷的二维 qNMR 方法。利用带选择性的 HSQC 和特征 10-10'键的交叉相关，我们在五分钟内定量了决定价值的二蒽酮类化合物的总量，从而使该方法不仅快速，而且具有特异性和稳定性指示。方法验证表明该方法具有极好的准确性（回收率为 98.5%至 103%）、精密度（RSD 值为 3.1%）和重复性（2.2%），并证明了 2D qNMR 在药用植物质量控制中的潜力。在第二种方法中，用二维 qNMR 对番泻苷 A、B 和 A 进行了单一分析，其测量时间（31 分钟）可接受，主要泻药番泻苷 A 和 B 的准确性（93.8%）和重复性（5.4%和 5.6%）令人满意。然而，番泻苷 B 和 A 的精密度不理想，主要是由于这两种化合物的 HSQC 信号分辨率较低。
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