Simultaneous determination of naproxen, salicylic acid and acetylsalicylic acid by spectrofluorimetry using partial least-squares (PLS) multivariate calibration.
Simultaneous determination of naproxen, salicylic acid and acetylsalicylic acid by spectrofluorimetry using partial least-squares (PLS) multivariate calibration.
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DOI：
10.1016/s0039-9140(98)00268-9
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发表时间：
1999-02
期刊：
影响因子：
6.1
通讯作者：
A. Navalón;R. Blanc;M. Olmo;J. Vílchez
中科院分区：
文献类型：
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作者：
A. Navalón;R. Blanc;M. Olmo;J. Vílchez
在300 ~ 520 nm波长范围内记录荧光发射光谱，以290 nm为激发波长，测定了萘普生、水杨酸和乙酰水杨酸的含量。这些化合物的激发-发射光谱是强烈重叠的，这不允许它们在没有通过常规方法预先分离的情况下直接测定。在这里，提出了一种方法，通过使用全光谱多元校正方法，偏最小二乘法（PLS）的这些化学品的测定。设计了18个样品的实验校准矩阵。萘普生的浓度范围为0.1 - 1.0 μg ml− 1，水杨酸的浓度范围为0.5 - 5.0 μg ml− 1，乙酰水杨酸的浓度范围为2.0 - 12.0 μg ml− 1。交叉验证方法用于选择因子的数量。为了检查所提出的方法的准确性，使用PLS-1获得的优化模型，应用于测定这些化合物的药物和人血清样品中预先掺入不同量的每种化学品。
Determination of naproxen, salicylic acid and acetylsalicylic acid has been carried out in mixtures of up to three components by recording emission fluorescence spectra between 300 and 520 nm with an excitation wavelength of 290 nm. The excitation–emission spectra of these compounds are strongly overlapped, which does not permit their direct determination without previous separation by conventional methodologies. Here, a method is proposed for the determination of these chemicals by the use of a full-spectrum multivariate calibration method, partial least-squares (PLS). The experimental calibration matrix was designed with 18 samples. The concentrations were varied between 0.1 and 1.0 μg ml−1for naproxen, 0.5 and 5.0 μg ml−1for salicylic acid and from 2.0 to 12.0 μg ml−1for acetylsalicylic acid. The cross-validation method was used to select the number of factors. To check the accuracy of the proposed method, the optimized model, obtained using PLS-1, was applied to the determination of these compounds in pharmaceuticals and human serum samples previously spiked with different amounts of each chemical.