title: Fluorimetric determination of sulphaguanidine and sulphamethoxazole by host-guest complexation in beta-cyclodextrin and partial least squares calibration.
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.
authors: Department of Analytical Chemistry, Faculty of Sciences, University of Extremadura, 06071 Badajoz, Spain. nielene@unex.es
authors: N Mora
authors: NM
authors: Diez
authors: A Muñoz
authors: AM
authors: de la Peña
authors: M C Mahedero
authors: MC
authors: García
authors: D Bohoyo
authors: DB
authors: Gil
authors: F
authors: F
authors: Cañada-Cañada
mesh_terms: D002021:Buffers; D002138:Calibration; D006801:Humans; D006863:Hydrogen-Ion Concentration; D057927:Hydrophobic and Hydrophilic Interactions; D016018:Least-Squares Analysis; D008958:Models, Molecular; D013050:Spectrometry, Fluorescence / Q000379:methods*; D013056:Spectrophotometry, Ultraviolet / Q000379:methods; D013414:Sulfaguanidine / Q000032:analysis* / Q000737:chemistry / Q000652:urine; D013420:Sulfamethoxazole / Q000032:analysis* / Q000737:chemistry / Q000652:urine; D013424:Sulfanilamides / Q000737:chemistry; D013816:Thermodynamics; D047392:beta-Cyclodextrins / Q000737:chemistry*
chemical_list: D002021:Buffers; D013424:Sulfanilamides; D047392:beta-Cyclodextrins; D013414:Sulfaguanidine; D013420:Sulfamethoxazole; C031215:betadex