RESUMO
Acotiamide hydrochloride trihydrate is a novel gastroprokinetic drug which has been recently approved for the treatment of patients with functional dyspepsia. This study presents the first reported to investigate the fluorimetric behavior of acotiamide hydrochloride trihydrate in the presence of its oxidative degradation product. All variables that affect fluorescence intensity were studied and optimized. The described method involved the measurement of native fluorescence of the drug in ethanol at 404 nm after excitation at 326 nm. Calibration plot was found to be linear over the concentration range 0.1-0.9 µg/ml. The specificity of the method has been tested via selective determination of the studied drug in its synthetic mixtures with its degradation product. The proposed method has been successfully applied to the analysis of the drug in its new pharmaceutical dosage form and the results have been statistically compared with the reported HPLC method showing no significant differences by applying t-test and F-test.
Assuntos
Benzamidas/análise , Fármacos Gastrointestinais/análise , Tiazóis/análise , Benzamidas/metabolismo , Cromatografia Líquida de Alta Pressão , Fármacos Gastrointestinais/metabolismo , Concentração de Íons de Hidrogênio , Estrutura Molecular , Oxirredução , Espectrometria de Fluorescência , Tensoativos/química , Tiazóis/metabolismoRESUMO
A reversed-phase HPLC method (RP-HPLC) with UV detection was developed and validated for the quantitative determination of cefprozil, a second-generation cephalosporin. Due to ß-lactam ring instability under alkaline conditions, this RP-HPLC method was applied for the determination of cefprozil in the presence of its possible degradation product. The interactions that govern the separation process with stationary phase were investigated at both molecular and quantum mechanical levels. Moreover, electrostatic potential maps were generated to determine the sites of interaction with mobile phase. The suggested method was validated in compliance with International Conference on Harmonization guidelines and successfully applied for the determination of cefprozil in its commercial pharmaceutical formulation.
Assuntos
Cefalosporinas/análise , Cromatografia de Fase Reversa , Interações Hidrofóbicas e Hidrofílicas , Modelos Químicos , Piperazinas/análise , Piperazinas/síntese química , Teoria Quântica , Hidróxido de Sódio/química , Espectrofotometria Ultravioleta , CefprozilRESUMO
For the first time, a new variable selection method based on swarm intelligence namely firefly algorithm is coupled with three different multivariate calibration models namely, concentration residual augmented classical least squares, artificial neural network and support vector regression in UV spectral data. A comparative study between the firefly algorithm and the well-known genetic algorithm was developed. The discussion revealed the superiority of using this new powerful algorithm over the well-known genetic algorithm. Moreover, different statistical tests were performed and no significant differences were found between all the models regarding their predictabilities. This ensures that simpler and faster models were obtained without any deterioration of the quality of the calibration.
RESUMO
Three different spectrophotometric methods were applied for the quantitative analysis of flucloxacillin and amoxicillin in their binary mixture, namely, ratio subtraction, absorbance subtraction and amplitude modulation. A comparative study was done listing the advantages and the disadvantages of each method. All the methods were validated according to the ICH guidelines and the obtained accuracy, precision and repeatability were found to be within the acceptable limits. The selectivity of the proposed methods was tested using laboratory prepared mixtures and assessed by applying the standard addition technique. So, they can be used for the routine analysis of flucloxacillin and amoxicillin in their binary mixtures.
Assuntos
Amoxicilina/análise , Antibacterianos/análise , Floxacilina/análise , Espectrofotometria/métodos , Análise de Variância , Cápsulas , Combinação de Medicamentos , Limite de DetecçãoRESUMO
Four rapid, simple, accurate and precise spectrophotometric methods were used for the determination of ciprofloxacin in the presence of its acidic degradation product. The methods under study are ratio derivative, ratio difference, mean centering and dual wavelength. All the methods were validated according to the ICH guidelines and the obtained accuracy, precision and repeatability were found to be within the acceptable limits. The selectivity of the proposed methods was tested using laboratory prepared mixtures and assessed by applying the standard addition technique. So, they can be used for the routine analysis of ciprofloxacin in quality-control laboratories.
Assuntos
Antibacterianos/análise , Ciprofloxacina/análise , Espectrofotometria/métodos , Ácidos/análise , Análise de Variância , Estabilidade de Medicamentos , Limite de Detecção , Reprodutibilidade dos Testes , Espectrofotometria/economiaRESUMO
Three simple, specific, accurate and precise spectrophotometric methods were developed for the determination of cefprozil (CZ) in the presence of its alkaline induced degradation product (DCZ). The first method was the bivariate method, while the two other multivariate methods were partial least squares (PLS) and spectral residual augmented classical least squares (SRACLS). The multivariate methods were applied with and without variable selection procedure (genetic algorithm GA). These methods were tested by analyzing laboratory prepared mixtures of the above drug with its alkaline induced degradation product and they were applied to its commercial pharmaceutical products.
Assuntos
Antibacterianos/química , Cefalosporinas/química , Espectrofotometria/métodos , Algoritmos , Álcalis/química , Estabilidade de Medicamentos , Análise dos Mínimos Quadrados , Análise Multivariada , CefprozilRESUMO
Four rapid, simple, accurate and precise spectrophotometric methods were used for the determination of ciprofloxacin in the presence of metronidazole as interference. The methods under study are area under the curve, simultaneous equation in addition to smart signal processing techniques of manipulating ratio spectra namely Savitsky-Golay filters and continuous wavelet transform. All the methods were validated according to the ICH guidelines where accuracy, precision and repeatability were found to be within the acceptable limits. The selectivity of the proposed methods was tested using laboratory prepared mixtures and assessed by applying the standard addition technique. So, they can therefore be used for the routine analysis of ciprofloxacin in quality-control laboratories.
Assuntos
Anti-Infecciosos/análise , Ciprofloxacina/análise , Metronidazol/análise , Espectrofotometria/métodos , Antibacterianos/análise , Limite de Detecção , Espectrofotometria/economia , Análise de OndaletasRESUMO
Different chemometric models were applied for the quantitative analysis of amoxicillin (AMX), and flucloxacillin (FLX) in their binary mixtures, namely, partial least squares (PLS), spectral residual augmented classical least squares (SRACLS), concentration residual augmented classical least squares (CRACLS) and artificial neural networks (ANNs). All methods were applied with and without variable selection procedure (genetic algorithm GA). The methods were used for the quantitative analysis of the drugs in laboratory prepared mixtures and real market sample via handling the UV spectral data. Robust and simpler models were obtained by applying GA. The proposed methods were found to be rapid, simple and required no preliminary separation steps.
Assuntos
Amoxicilina/análise , Antibacterianos/análise , Floxacilina/análise , Espectrofotometria Ultravioleta/métodos , Algoritmos , Formas de Dosagem , Combinação de Medicamentos , Análise dos Mínimos Quadrados , Redes Neurais de Computação , Espectrofotometria Ultravioleta/economiaRESUMO
Four simple, accurate and precise stability-indicating spectrophotometric methods manipulating ratio spectra were developed and validated for simultaneous determination of Cefprozil (CZ) and its alkaline-induced degradation product (DCZ) without prior separation namely; ratio difference, mean centering, derivative ratio using Savitsky-Golay filter and continuous wavelet transform. The accuracy, precision and linearity ranges of the proposed methods were determined. The methods were validated and the specificity was assessed by analyzing synthetic mixtures containing the drug and its degradate. The four methods were applied for the determination of the cited drug in tablets and the obtained results were statistically compared with those of a reported method. The comparison showed that there are no significant differences between the proposed methods and the reported method regarding both accuracy and precision.