偏最小二乘紫外分光光度法同时测定丁烯二酸的顺反异构体

将偏最小二乘法用于紫外分光光度分析,在pH=1.4的磷酸溶液中,同时测定了丁烯二酸的顺、反异构体。确定了测定的最佳波长范围为190～268nm;测得23个混合标样的吸光度值用于建立模型,顺、反丁烯二酸的浓度范围为3.0～14.0mg/L和1.0～13.0mg/L。所建立的测定二者模型的相关系数分别为0.9951和0.9983;平均回收率分别为100.8%和100.7%;均方根误差(RMSE)分别为0.3667和0.2233;预测相对误差(REP)分别为5.05%和3.49%。对3个批次反丁烯二酸样品的测定结果与高效液相色谱法的测定结果进行比较,经成对t检验表明,两种方法的测定结果无显著性差异。

Simultaneous Determination of cis-and trans-Butendioic Acid by Partial Least Squares-Ultraviolet Spectrophotometry

The calibration models were established for the determination of cis-and trans-butendioic acid by partial least squares(PLS)and ultraviolet spectrophotometry.The absorption spectra in the range of 190-268 nm for 23 different mixtures of butendioic acid isomers in phosphoric acid solution(pH=1.4)were used as calibration set.Correlation coefficients of the models for cis-and trans-butendioic acid were 0.9951 and 0.9983,the mean recoveries were 100.8% and 100.7%,the root mean square errors of prediction(RMSE)were 0.3667 and 0.2233,and the relative error of prediction(REP)were 3.49% and 5.05% in the predicted range of 1.0-13.0 and 3.0-14.0 mg/L,respectively.By statistical signification test,the results of the determination were compared with those of HPLC without significant difference at 0.05 level.The proposed method has been applied to the simultaneous determination of cis-and trans-butendioic acid in real samples with satisfactory results.