A simple solid phase spectrofluorimetric method combined with flow analysis for the rapid determination of salicylamide and salicylic acid in pharmaceutical samples

Abstract

A new, sensitive and very simple spectrofluorimetric biparameter sensor is described for the determination of salicylamide and/or salicylic acid in pharmaceutical preparations. The method integrates the transitory retention and fluorescence detection of both compounds on Sephadex QAE A-25 resin packed into a conventional flow-through cell. A monochannel manifold with two alternative carriers is used. At pH 2.0 (first carrier) salicylic acid is selectively retained on the solid support and after developing the analytical signal it is desorbed. At pH 11.0 (second carrier) both salicylic acid and salicylamide are simultaneously and transitorily retained on the solid, the analytical signal now corresponding to both analytes. The monochromators were tuned at 260 (excitation) and 415 (emission) nm, respectively. The calibration graph for salicylamide is linear over the range 0.01 to 0.32 μg mL^–1 and for salicylic acid from 0.04 to 1.0 μg mL^–1 in the presence of each other. The relative standard deviation and the sampling frequency for the determination of salicylamide (0.20 μg mL^–1) and salicylic acid (0.50 μg mL^–1) were 1.1% and 35 h^–1, and 0.9% and 45 h^–1, respectively. Good results on application to individual determination or mixture resolution in pharmaceutical samples testify to the usefulness of the proposed sensor.