Direct determination of closely overlapping drug mixtures of diflunisal and salicylic acid in serum by means of derivative matrix isopotential synchronous fluorescence spectrometry
Direct determination of closely overlapping drug mixtures of diflunisal and salicylic acid in serum by means of derivative matrix isopotential synchronous fluorescence spectrometry
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DOI：
10.1016/j.aca.2006.10.009
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发表时间：
2007-01
影响因子：
6.2
通讯作者：
J. M. Pulgarín;A. A. Molina-A.;P. F. Lopez;I. S. Robles
中科院分区：
文献类型：
--
作者：
J. M. Pulgarín;A. A. Molina-A.;P. F. Lopez;I. S. Robles
本文提出了一种同时测定血清中两种抗炎药的直接荧光法。基质等电位同步荧光（MISF）和一阶导数技术相结合，提供了良好的分析结果，并允许同时测定二氟尼柳和水杨酸在人血清中。通过计算血清溶液三维荧光光谱中的等势轨迹获得MISF光谱。在光谱轮廓中，轨迹被认为是通过两种化合物的荧光最大值的线的部分，确保灵敏度水平与不存在背景荧光的直接测定的灵敏度水平相似。使用由0.1M磷酸二氢钠缓冲液提供的pH 7.2在水中进行分析。将血清样品稀释100倍，并在二氟尼柳和水杨酸浓度高达800 ngmL −1时提供线性校准图。通过方差分析检查分析信号的良好性。在不存在和存在可变量的其他分析物的情况下，对整个校准范围内记录的信号进行三次校准。将单个校准和斜率之间的差异与单个校准内的差异进行比较。根据结果，二氟尼柳和水杨酸可以在彼此存在的情况下准确定量。根据克莱顿的计算，二氟尼柳和水杨酸的检测限分别为36.8和37.3 ngmL − 1，克莱顿使用整个校准曲线的误差传播和非集中安全因子。
A direct method for the simultaneous fluorimetric determination of two anti-inflammatory drugs in serum is proposed. The combination of matrix isopotential synchronous fluorescence (MISF) and first derivative technique provides good analytical results and permits the simultaneous determination of diflunisal and salicylic acid in human serum. MISF spectra are obtained by calculating the isopotential trajectory in the three-dimensional fluorescence spectrum for a serum solution. In the spectral contour, the trajectory is taken to be the portion of the line that passes by the fluorescence maxima of both compounds ensuring a sensitivity level similar to that of a direct determination in absence of background fluorescence. Analysis was carried out in water using a pH of 7.2 provides by 0.1M sodium dihydrogen phosphate buffer. Serum samples are diluted 100 times and provide linear calibration plots at diflunisal and salicylic acid concentrations up to 800ngmL−1. The goodness of the analytical signal was checked by using variance analysis. Signals recorded throughout the calibration range were subjected to three calibrations per each analyte, both in the absence and in the presence of variable amounts of the other analyte. Differences between individual calibrations and slopes were compared with those within individual calibrations. Based on the results, diflunisal and salicylic acid can be accurately quantified in the presence of each other. The limit of detection calculated according to Clayton who uses error propagation throughout the calibration curve and a non-centralized security factor was 36.8 and 37.3ngmL−1for diflunisal and salicylic acid, respectively.