Direct determination of closely overlapping drug mixtures of diflunisal and salicylic acid in serum by means of derivative matrix isopotential synchronous fluorescence spectrometry.
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 0.1 M sodium dihydrogen phosphate buffer. Serum samples are diluted 100 times and provide linear calibration plots at diflunisal and salicylic acid concentrations up to 800 ng mL(-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 37.3 ng mL(-1) for diflunisal and salicylic acid, respectively.
Murillo Pulgarín
J A
JA
Department of Analytical Chemistry and Foods Technology, University Castilla-La Mancha, 13071 Ciudad Real, Spain. joseantonio.murillo@uclm.es
Alañón Molina
A
A
Fernández López
P
P
Sánchez-Ferrer Robles
I
I
D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000097:blood; D004061:Diflunisal / Q000097:blood*; D006801:Humans; D004364:Pharmaceutical Preparations / Q000737:chemistry*; D020156:Salicylic Acid / Q000097:blood*; D012680:Sensitivity and Specificity; D012984:Software; D013050:Spectrometry, Fluorescence / Q000379:methods
D000894:Anti-Inflammatory Agents, Non-Steroidal; D004364:Pharmaceutical Preparations; D004061:Diflunisal; D020156:Salicylic Acid