摘要
探讨在新药基准物质的确定过程中 ,利用核磁共振法测定药物绝对含量的可行性。以环丙沙星、安妥沙星、卡德沙星、加替沙星、左氧氟沙星、氧氟沙星、诺氟沙星、依诺沙星和洛美沙星 9种喹诺酮类抗生素化学对照品为例 ,其中安妥沙星和卡德沙星为国家一类新药。采用重水、氘代二甲基亚砜或氢氧化钠的重水溶液为溶剂 ,对苯二酚或顺丁烯二酸为内标 ,用喹诺酮母核上的质子峰进行定量 ,以内标法和外标法计算含量。核磁共振法测定结果与各对照品标签示值的误差约为 1 % ,内标法和外标法的计算结果一致。该方法专属、准确、简便、快速 。
This article discussed the feasibility of determining the content of reference substance by 1H nuclear magnetic resonance spectroscopy (NMR). 9 reference substances of quinolone antibiotics were chosen as examples, such as ciprofloxacin, antofloxacin, caderofloxacin, gatifloxacin, L ofloxacin, ofloxacin, norfloxacin, enoxacin, lomefloxacin. D 2O, D 6 dimethyl sulfoxide (DMSO), or 0.3 mol/L NaOH in D 2O solution was used as solvent. Hydroquinone and maleic acid were selected as internal standard. By measuring the selected proton peak intensity, the quantitative analysis of samples was achieved. The difference between the result of NMR method and labelled content was about 1%. The results came from the internal standard method were same as those of external standard one. This method is specificity, rapid, accurate, simple, and it is suitable for the quantitative determination of the reference substance content.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2004年第4期451-455,共5页
Chinese Journal of Analytical Chemistry
