RESUMO
BACKGROUND: Vinpocetine has been prescribed for the treatment of ischemic brain diseases for many years. The drug, which has side effects such as headache, flushing, and decreased blood pressure, is not found in nature, but it can be synthesized by several approaches. OBJECTIVE: A simple, rapid, selective, stability-indicating high-performance liquid chromatographic (HPLC) method was developed for the simultaneous estimation of vinpocetine and their potential impurities in a tablet formulation. METHOD: Optimum HPLC conditions were tried to be determined by a statistical experimental design method. The proposed method was validated as per the ICH guidelines. Stress study was used to demonstrate the stability-indicating ability of the developed method in the quantification of vinpocetine and potential impurities within the same run. RESULTS: According to multiresponse optimization using the Derringer's desirability function, the mobile phase consisted of an acetonitrile-phosphate buffer (pH 6.0) in the ratio of 65:35 (v/v) at a flow rate of 1.7 mL/min. Significant degradations were observed for the drug product under acid hydrolysis and alkali hydrolysis. The new method showed reasonable detection and quantification limits with good selectivity, precision, linearity, and recovery. CONCLUSIONS: These validation results have shown that this method is suitable for quantitative determination of vinpocetine and its impurities in quality control laboratories. HIGHLIGHTS: A reliable and rapid HPLC method optimized with response surface methodology and multiresponse optimization based on Derringer's desirability function was developed for the simultaneous analysis of vinpocetine and its impurities in a tablet formulation.
Assuntos
Projetos de Pesquisa , Cromatografia Líquida de Alta Pressão/métodos , Reprodutibilidade dos Testes , Comprimidos , Alcaloides de VincaRESUMO
BACKGROUND: In many countries, the levels of synthetic food additives causing harm to humans have been determined and their use has been controlled by legal regulations. Sensitive, accurate and low-cost analysis methods are required for food additive determination. OBJECTIVE: In this study, a fast high performance liquid chromatography-diode array detection (HPLC-DAD) analytical methodology for quantification of sodium benzoate, potassium sorbate, ponceau 4R, and carmoisine in a beverage was proposed. METHODS: Partial least squares (PLS) and principal component regression (PCR) multivariate calibration methods applied to chromatograms with overlapped peaks were used to establish a green and smart method with short isocratic elution. A series of synthetic solutions including different concentrations of analytes were used to test the prediction ability of the developed methods. CONCLUSIONS: The average recoveries for all target analytes were in the range of 98.27-101.37% with average relative prediction errors of less than 3%. The proposed chemometrics-assisted HPLC-DAD methods were implemented to a beverage successfully. Analysis results from sodium benzoate, potassium sorbate, ponceau 4R, and carmoisine in a beverage by PLS-2 and PCR were statistically compared with conventional HPLC. HIGHLIGHTS: The HPLC methods coupled with the PLS-2 and PCR algorithm could provide a simple, quick and accurate strategy for simultaneous determination of sodium benzoate, potassium sorbate, ponceau 4R, and carmoisine in a beverage sample.
Assuntos
Bebidas , Aditivos Alimentares , Bebidas/análise , Calibragem , Cromatografia Líquida de Alta Pressão , Humanos , Análise dos Mínimos QuadradosRESUMO
Background: Preservatives and colorants in pharmaceutical products may be highly toxic, especially for sensitive individuals, when they are used in excessive amounts. In this context, sensitive and non-labor-intensive analytical methods with short analysis time for simultaneous quantification of these additive substances in drugs can meet all requirements in quality control laboratories. Objective: The aim of the study was to develop a simultaneous HPLC method for the analysis of pseudoephedrine HCl and guaifenesin, along with preservatives, methyl paraben and propyl paraben, and colorants, ponceau 4R and sunset yellow, in a syrup sample. Methods: Optimum conditions of HPLC separation were determined by Box-Behnken experimental design. Four independent variables of the separation were pH (6.0, 6.5, and 7.0) and flow rate of the mobile phase (2.0, 2.2, and 2.4 mL/min) and mobile phase ratios for the first and second gradient elutions (75, 80, and 85% for Gradient 1 and 50, 55, and 60% for Gradient 2 in terms of phosphate buffer percent, respectively). Results: The optimum conditions were found to be pH, 6.3; flow rate, 2.4 mL/min; and mobile phase ratios (phosphate buffer-acetonitrile) for Gradient 1 and 2, 85+15 (v/v) and 60+40 (v/v), respectively. Conclusions: Simultaneous analysis of all compounds was achieved by using this HPLC method with a short run time below 10 min. Highlights: This simple, rapid, and validated method is convenient and applicable for routine analysis of pharmaceutical products having similar composition without the need for any extraction step.
Assuntos
Compostos Azo/análise , Cromatografia Líquida de Alta Pressão/métodos , Guaifenesina/análise , Naftalenossulfonatos/análise , Parabenos/análise , Pseudoefedrina/análise , Corantes/análise , Conservantes Farmacêuticos/análiseRESUMO
In this study, development and validation of a HPLC method was described for simultaneous determination of potassium sorbate, sodium benzoate, quinoline yellow and sunset yellow. A Box-Behnken design using three variables at three levels was employed to determine the optimum conditions of chromatographic separation: pH of mobile phase, 6.0-7.0; flow rate, 0.8-1.2 mL min(-1) and the ratio of mobile phase composed of a 0.025 M sodium acetate/acetic acid buffer, 80-90%. Resolution was chosen as a response. The optimized method was validated for linearity, the limits of detection and quantification, accuracy, precision and stability. All the validation parameters were within the acceptance range. The applicability of the developed method to the determination of these food additives in commercial lemonade and lemon sauce samples was successfully demonstrated.
Assuntos
Compostos Azo/análise , Cromatografia Líquida de Alta Pressão , Análise de Alimentos/métodos , Quinolinas/análise , Benzoato de Sódio/análise , Ácido Sórbico/análise , Bebidas/análise , Projetos de PesquisaRESUMO
Box-Behnken design was applied to optimize high performance liquid chromatography (HPLC) conditions for the simultaneous determination of potassium sorbate, sodium benzoate, carmoisine, allura red, ponceau 4R, and caffeine in commercial soft drinks. The experimental variables chosen were pH (6.0-7.0), flow rate (1.0-1.4 mL/min), and mobile phase ratio (85-95% acetate buffer). Resolution values of all peak pairs were used as a response. Stationary phase was Inertsil OctaDecylSilane- (ODS-) 3V reverse phase column (250 × 4.6 mm, 5 µm) dimensions. The detection was performed at 230 nm. Optimal values were found 6.0 pH, 1.0 mL/min flow rate, and 95% mobile phase ratio for the method which was validated by calculating the linearity (r (2) > 0.9962), accuracy (recoveries ≥ 95.75%), precision (intraday variation ≤ 1.923%, interday variation ≤ 1.950%), limits of detection (LODs), and limits of quantification (LOQs) parameters. LODs and LOQs for analytes were in the range of 0.10-0.19 µg/mL and 0.33-0.63 µg/mL, respectively. The proposed method was applied successfully for the simultaneous determination of the mixtures of five food additives and caffeine in soft drinks.
RESUMO
A simple and rapid analytical procedure was proposed for the determination of chromatographic peaks by means of partial least squares multivariate calibration (PLS) of high-performance liquid chromatography with diode array detection (HPLC-DAD). The method is exemplified with analysis of quaternary mixtures of potassium guaiacolsulfonate (PG), guaifenesin (GU), diphenhydramine HCI (DP) and carbetapentane citrate (CP) in syrup preparations. In this method, the area does not need to be directly measured and predictions are more accurate. Though the chromatographic and spectral peaks of the analytes were heavily overlapped and interferents coeluted with the compounds studied, good recoveries of analytes could be obtained with HPLC-DAD coupled with PLS calibration. This method was tested by analyzing the synthetic mixture of PG, GU, DP and CP. As a comparison method, a classsical HPLC method was used. The proposed methods were applied to syrups samples containing four drugs and the obtained results were statistically compared with each other. Finally, the main advantage of HPLC-PLS method over the classical HPLC method tried to emphasized as the using of simple mobile phase, shorter analysis time and no use of internal standard and gradient elution.