Tachibana S, Nishiura S, Ishida S, Kakehi K, Honda S
Kinki University Hospital, Osaka-sayama, Japan.
Chem Pharm Bull (Tokyo). 1990 Sep;38(9):2503-6. doi: 10.1248/cpb.38.2503.
The quality of commercial heparin injections was examined by 400-MHz proton nuclear magnetic resonance (1H-NMR) spectroscopy using several measuring modes. The signals of the N-acetyl protons, as well as the sugar-ring protons, attached to the sulfamino and sulfato group-bearing carbons could be easily distinguished from other proton signals and quantified. Measuring at a high temperature (60 degrees C) enabled clear isolation of the H-5 proton signal in the sulphated iduronic acid residue (Is-5) from other proton signals including that of water. The heparin contents of various heparin injections were estimated by using this signal as an index. However, the signal intensity was not parallel with anticoagulant activity. On the other hand, the N-acetyl proton signal was highly correlated to anticoagulant activity. The present method was also useful for concurrent identification of additives in heparin injections.
使用多种测量模式，通过400兆赫质子核磁共振（1H-NMR）光谱法对商业肝素注射液的质量进行了检测。与含磺氨基和硫酸根基团的碳相连的N-乙酰基质子以及糖环质子的信号能够轻易地与其他质子信号区分开来并进行定量分析。在高温（60摄氏度）下测量能够将硫酸化艾杜糖醛酸残基（Is-5）中的H-5质子信号与包括水信号在内的其他质子信号清晰地分离出来。以该信号为指标估算了各种肝素注射液中的肝素含量。然而，信号强度与抗凝活性并不平行。另一方面，N-乙酰基质子信号与抗凝活性高度相关。本方法对于同时鉴定肝素注射液中的添加剂也很有用。
