Synchronous fluorimetric determination of salicylic acid and diflunisal in human serum using partial least-squares calibration

被引:32
作者
delaPena, AM
Moreno, MD
DuranMeras, I
Salinas, F
机构
[1] Department of Analytical Chemistry, University of Extremadura
关键词
diflunisal; partial least-squares; salicylic acid; synchronous fluorimetry;
D O I
10.1016/0039-9140(96)01910-8
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
The simultaneous determination of salicylic acid and diflunisal in human serum has been accomplished by synchronous fluorimetry, in combination with partial least-squares multivariate calibration. The total luminescence information of the analytes has been used to optimize the spectral data set for the calibration, by analysis of the three-dimensional excitation-emission matrices. The synchronous spectrum, maintaining a constant difference of Delta lambda = 128 nm between the emission and excitation wavelengths, has been selected as optimum to perform the determination. The method is based on the fluorescence of these compounds in chloroform containing 1% (v/v) acetic acid. Serum samples are treated with trichloroacetic acid to remove the proteins, and both analytes are extracted into chloroform-1% (v/v) acetic acid prior to the determination. For concentrations ranging from 60-240 mu g ml(-1) of each drug, analytical recoveries range from 96% to 103% for salicylic acid and from 97% to 105% for diflunisal.
引用
收藏
页码:1349 / 1356
页数:8
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