Abstract
The host-guest inclusion complexes of sulphamethoxazole (SMTX) and sulphaguanidine (SGN) with β-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 μg mL−1 for SMTX and 1.0 μg 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.
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Acknowledgements
Financial support provided by the Consejería de Infraestructuras y Desarrollo Tecnológico de la Junta de Extremadura and Fondos Feder (Project 2PR04A007) is greatly acknowledged. Diego Bohoyo Gil is grateful to the Consejería de Educación, Ciencia y Tecnología de la Junta de Extremadura for a fellowship (DOE 21/06/01). The authors are grateful to Diego Airado Rodríguez for his help in the validation of the proposed procedure by the liquid chromatographic method.
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Diez, N.M., de la Peña, A.M., García, M.C.M. et al. Fluorimetric Determination of Sulphaguanidine and Sulphamethoxazole by Host-Guest Complexation in β-Cyclodextrin and Partial Least Squares Calibration. J Fluoresc 17, 309–318 (2007). https://doi.org/10.1007/s10895-007-0174-4
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DOI: https://doi.org/10.1007/s10895-007-0174-4