Kirchhoefer R D
J Pharm Sci. 1980 Oct;69(10):1188-91. doi: 10.1002/jps.2600691018.
A quantitative high-pressure liquid chromatographic method that uses a reversed-phase column coupled to UV and fluorescence detectors was developed to determine aspirin and salicylic acid in bulk aspirin and in plain, buffered, and enteric-coated tablets. The aspirin was dissolved, filtered, and injected into the chromatograph. The UV absorbance of aspirin was determined at 254 nm, and the fluorescence of salicylic acid was measured at 425 nm. Excipients and impurities did not interfere. Recoveries of 100% were obtained for aspirin and salicylic acid from simulated tablet formulations. Results obtained by the USP XIX procedure and the proposed method were compared. The coefficient of variation for the aspirin analysis was 0.59%; for salicylic acid, it was 1.69%. The rate of hydrolysis of aspirin to salicylic acid in the solvents used was < 0.05%/hr.
开发了一种定量高压液相色谱法,该方法使用与紫外和荧光检测器相连的反相柱,用于测定原料药阿司匹林以及普通片、缓冲片和肠溶片中的阿司匹林和水杨酸。将阿司匹林溶解、过滤后注入色谱仪。在254nm处测定阿司匹林的紫外吸光度,在425nm处测量水杨酸的荧光。辅料和杂质不产生干扰。从模拟片剂配方中回收的阿司匹林和水杨酸的回收率为100%。比较了美国药典第十九版方法和所提出方法的结果。阿司匹林分析的变异系数为0.59%;水杨酸的变异系数为1.69%。所用溶剂中阿司匹林水解为水杨酸的速率<0.05%/小时。