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1.
Luminescence ; 31(3): 856-64, 2016 May.
Artigo em Inglês | MEDLINE | ID: mdl-26456088

RESUMO

The aim of this work is to optimize a spectrofluorimetric method for the determination of cefdinir (CFN) using the Taguchi method. The proposed method is based on the oxidative coupling reaction of CFN and cerium(IV) sulfate. The quenching effect of CFN on the fluorescence of the produced cerous ions is measured at an emission wavelength (λ(em)) of 358 nm after excitation (λ(ex)) at 301 nm. The Taguchi orthogonal array L9 (3(4)) was designed to determine the optimum reaction conditions. The results were analyzed using the signal-to-noise (S/N) ratio and analysis of variance (ANOVA). The optimal experimental conditions obtained from this study were 1 mL of 0.2% MBTH, 0.4 mL of 0.25% Ce(IV), a reaction time of 10 min and methanol as the diluting solvent. The calibration plot displayed a good linear relationship over a range of 0.5-10.0 µg/mL. The proposed method was successfully applied to the determination of CFN in bulk powder and pharmaceutical dosage forms. The results are in good agreement with those obtained using the comparison method. Finally, the Taguchi method provided a systematic and efficient methodology for this optimization, with considerably less effort than would be required for other optimizations techniques.


Assuntos
Cefalosporinas/análise , Cério/química , Projetos de Pesquisa , Sulfatos/química , Cefdinir , Fluorescência , Estrutura Molecular , Espectrometria de Fluorescência
2.
J Sep Sci ; 38(6): 901-8, 2015 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-25565679

RESUMO

The aim of the present study was to optimize a microemulsion liquid chromatography method for the simultaneous determination of norfloxacin and tinidazole binary mixture using a chemometric protocol. Optimization experiments were conducted through a process of screening and optimization. A 2(7-4) fractional factorial design was used as screening design. While the location of optimum conditions was established by applying Derringer's desirability function. The optimal mobile phase composition was predicted to be: 3.5% w/v SDS, 10.03% v/v 1-propanol, 0.5% v/v 1-octanol, and 0.3% triethylamine in 0.02 M phosphoric acid at pH 6.5. The mobile phase was delivered isocratically at a flow rate of 1 mL/min with UV detection at 290 nm. Tinidazole and norfloxacin were eluted with retention times of 1.8 and 5.8 min, respectively. The calibration plots displayed good linear relationships in the concentration ranges of 0.5-50 and 0.75-75 µg/mL for norfloxacin and tinidazole, respectively. The method was successfully applied for determination of both drugs in pharmaceutical dosage forms and real human plasma. Where the accuracy was proved by the low values of % error and high values of recovery, also the relative standard deviation for the results did not exceed 1.5%, proving the precision of the method.


Assuntos
Antibacterianos/sangue , Cromatografia Líquida de Alta Pressão/métodos , Norfloxacino/sangue , Tinidazol/sangue , Antibacterianos/química , Emulsões/química , Humanos , Norfloxacino/química , Plasma/química , Tinidazol/química
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