Li Chia-Ying, Lin Chung-Hua, Wu Tian-Shung
Department of Chemistry, National Cheng Kung University, Tainan, Taiwan.
Chem Pharm Bull (Tokyo). 2005 Mar;53(3):347-9. doi: 10.1248/cpb.53.347.
A quantitative analysis using (1)H-NMR has been developed for the determination of camptothecin derivatives and trigonelline in Nothapodytes foetida root, stems and leaves. In the region of delta 9.5-5.5, the signals of H-7 of camptothecin (1), H-10 of 9-methoxycamptothecin (2), H-19 of pumiloside (3) and H-2 of trigonelline (4), were well separated from each other in DMSO-d(6). The quantity of the compounds was calculated by the ratio of the intensity of each compound to the known amount of internal standard 3,4,5-trimethoxybenzaldehyde. These results were compared with the conventional HPLC method. The advantages of the method are that no reference compounds are required for calibration curves, the quantification could be directly realized on a crude extract, an overall profile of the preparation could be directly obtained, and a very significant time-gain could be achieved, in comparison to conventional HPLC methods, for instance.
已开发出一种使用(1)H-NMR的定量分析方法,用于测定印度马比木根、茎和叶中的喜树碱衍生物和胡芦巴碱。在δ 9.5 - 5.5区域,喜树碱(1)的H-7、9-甲氧基喜树碱(2)的H-10、喜果苷(3)的H-19和胡芦巴碱(4)的H-2信号在DMSO-d(6)中彼此分离良好。通过各化合物的强度与已知量内标3,4,5-三甲氧基苯甲醛的强度之比计算化合物的量。将这些结果与传统的HPLC方法进行比较。该方法的优点是校准曲线无需参考化合物,可直接在粗提取物上实现定量,可直接获得制剂的整体概况,并且与传统HPLC方法相比,例如可实现非常显著的时间节省。