导数光谱多组分标定法对阿司匹林、扑热息痛及水杨酸的同时测定

Simultaneous Determination of Aspirin,Paracetamol and Salicylic Acid by Derivative Spectrophotometric Multivariate Calibration Methods

采用导数光谱多组分标定法,根据中心合成设计建立标定集和预测集,将PLS和PCR应用于阿司匹林、扑热息痛及水杨酸混合物的零阶和一阶导数光谱,从而实现了混合物中各组分的同时测定。实验结果表明,阿司匹林、扑热息痛及水杨酸的吸收光谱严重重叠;由于各组分零交叉点重合,零交叉点比光谱-导数分光光度法无法同时测量混合物中各组分的含量;导数光谱多组分标定法能有效地避免线性范围内各组分零交叉点的重合,预测集中各组分的平均相对误差在3.6%以内,平均回收率均为101%,且具有良好的灵敏度;实际药品中各组分具有准确的预测值。导数光谱多组分标定法可在药物合成和质量检测时准确、有效地同时测定混合物中该3种组分的含量。

The calibration set and prediction set were configured according to the central composite design, then PLS and PCR were applied on zero and first order derivative spectra of the mixture of three components aspirin, paracetamol and salicylic acid. And the derivative spectrophotometric multivariate calibration methods were used for the simultaneous measurement of the mixture. The results showed that the absorption spectra of aspirin, paracetamol and salicylic acid overlapped seriously. Derivative-ratio spectrophotometry could not simultaneously measure the content of each component in the mixture since the zero-crossing points of the components overlapped. The derivative spectrophotometric multivariate calibration methods could effectively prevent the zero-crossing points of the individual components from coinciding in linear range. The average relative errors of all components in the prediction set were below 3.6% , and the average recoveries were 101%. Each component of the real pharmaceutical samples also had exact prediction results. With good sensitivity and the limit of detection, the derivative spectrophotometric multivariate calibration methods could be used to measure simultaneously the contents of the three components in drug synthesis and quality inspection.