基于子空间夹角判据监测阿司匹林合成体系中的水杨酸和阿司匹林

利用水杨酸、阿司匹林、乙酸酐和乙酸的多波长紫外光谱作为本底光谱库和样本光谱库,建立一种基于子空间夹角判据的快速定量分析阿司匹林合成体系中水杨酸和阿司匹林的方法。水杨酸、阿司匹林质量浓度范围分别在1.16～34.684,9.84～188.928μg/mL内,所测得水杨酸和阿司匹林检验集的R分别为0.999 7和0.999 1,RMSE分别为0.509 5,2.624 0μg/mL,效果优于普通波峰点最小二乘法和偏最小二乘法。水杨酸和阿司匹林的加标回收率在94.01%～106.44%之间,测定结果的相对标准偏差分别为3.45%和4.80%(n=7)。该方法可用于监测阿司匹林合成体系中的水杨酸和阿司匹林。

Monitoring Salicylic Acid and Aspirin in Synthesis Systems of Aspirin based on Subspace-Angle

Ultraviolet spectroscopy of salicylic acid,aspirin,acetic anhydride and acetic acid were used as background spectrum library and standard spectral library,and a rapid analytical method based on subspace-angle was developed for the quantitative determination of salicylic acid and aspirin in synthesis systems of aspirin. The results of R in test set of salicylic acid and aspirin were 0.999 7 and 0.999 1,respectively, and RMSE were 0.509 5μg/mL and 2.624 0μg/mL,respectively,in which the concentration range of salicylic acid and aspirin were 1.16-34.684μg/mL and 9.84-188.928μg/mL,respectively. It was better than OLS and PLS. The recoveries ranged from 94.01%to 106.44%,and the relative standard deviation of determination results was 3.45%and 4.80%（n=7） for salicylic acid and aspirin,respectively. The method was suitable to monitoring salicylic acid and aspirin in synthesis systems of aspirin.