ABSTRACT
The host-guest inclusion complexes of sulphamethoxazole (SMTX) and sulphaguanidine (SGN) with beta-cyclodextrin, in aqueous solutions, have been investigated. A 1:1 stoichiometry of the complexes was established, the association constants were calculated by different methods, and the influence of several chemical variables on the complexation processes were established. According to the results obtained, a spectrofluorimetric method for the determination of these sulphonamides has been proposed. The individual and binary mixtures of both sulphonamides have been determined in human urine samples, at representative therapeutic ranges, by application of a first-order multivariate calibration partial least squares (PLS-1) model. The calibration set was designed with 9 samples, containing different concentrations of the two sulphonamides, and 8 blank urine samples, with the aim of modelling the variability of the background. The concentration ranges for the sulphonamides were up to 0.5 microg mL(-1) for SMTX and 1.0 microg mL(-1) for SGN. Figures of merit as selectivity, analytical sensitivity and limit of detection (LOD) were also calculated. The proposed procedure was validated by comparing the obtained results with a HPLC method, with satisfactory results for the assayed method.
Subject(s)
Spectrometry, Fluorescence/methods , Sulfaguanidine/analysis , Sulfamethoxazole/analysis , beta-Cyclodextrins/chemistry , Buffers , Calibration , Humans , Hydrogen-Ion Concentration , Hydrophobic and Hydrophilic Interactions , Least-Squares Analysis , Models, Molecular , Spectrophotometry, Ultraviolet/methods , Sulfaguanidine/chemistry , Sulfaguanidine/urine , Sulfamethoxazole/chemistry , Sulfamethoxazole/urine , Sulfanilamides/chemistry , ThermodynamicsABSTRACT
This manuscript reports the usefulness of the determination of sulphathiazole (ST) using photochemically induced fluorescence (RTPF) and RTPF coupling with first derivative (D1-RTPF), and the determination of sulphanilamide (SAN) by meaning first derivative of the emission spectrum. By irradiating 5 min, with intense UV radiation, sulphathiazole, in ethanol:water 20:80 (v/v) solutions at pH 4.5-5.0, show fluorescence emission at 342 nm (lambdaex=251 nm). Under these conditions, a linear relation, fluorescence intensity-ST concentration, was found between 0.23 and 3.00 microg mL(-1) of ST. The method was applied for determining ST in a pharmaceutical drug. ST was also determined in honey by using the D1-RTPF signal, applying the standard addition method, and measuring at 324.8 nm. Under the same experimental conditions of pH and solvent, a fluorimetric method for determining SAN in presence of ST is proposed. Calibration graphs for SAN determination were established using the amplitude of the first derivative of the emission spectrum measured at 324.4 nm, as the analytical signal. This method has been applied to determining SAN in a pharmaceutical formulation.
