RESUMO
A new ion-pair high-performance liquid chromatography method with fluorescence detection was developed for the determination of nitidine and chelerythrine in Zanthoxylum nitidum. To optimize the separation of the two compounds in reversed-phase liquid chromatography, a response surface method (Box-Behnken designs) was used. Three important factors: concentration of ion pair agent, mobile phase composition and buffer pH, were studied for their contribution to the analytes' response, leading to a total of 17 experiments performed on a Kromasil C18 column. The experimental responses were fitted into a second-order polynomial to predict the best conditions. The optimal mobile phase conditions were predicted to be acetonitrile-sodium dodecyl sulphate (17.8 mM, 20 mM citric acid, pH 2.98, 57:43, v/v). The proposed method was validated according to International Conference on Harmonization guidelines and it is suggested to be appropriate for the routine quality control analysis of nitidine and chelerythrine in Zanthoxylum nitidum.
Assuntos
Benzofenantridinas/análise , Cromatografia Líquida de Alta Pressão/métodos , Zanthoxylum/química , Benzofenantridinas/química , Benzofenantridinas/isolamento & purificação , Estabilidade de Medicamentos , Extratos Vegetais/química , Reprodutibilidade dos Testes , Espectrometria de FluorescênciaRESUMO
The alkaloids in Zanthoxylum nitidum were identified by HPLC-DAD/ESI-Q-TOF-MS. Separation was performed on a Hanbon C18 column with acetonitrile (with 0.1% formic acid) and water(with 0.1% formic acid) as mobile phase. Based on the high-resolution mass information, MS/MS fragmentation behaviors and chemical components from literatures, 48 components were identified or tentatively characterized including 6 new compounds. This work could be useful for the quality control and further studies of the plant.
Assuntos
Alcaloides/química , Zanthoxylum/química , Cromatografia Líquida de Alta Pressão , Espectrometria de Massas por Ionização por Electrospray , Espectrometria de Massas por Ionização e Dessorção a Laser Assistida por MatrizRESUMO
OBJECTIVE: To optimize the process of extracting total flavonoids from Tagetes erecta. METHODS: The influential factors were extraction temperature, ethanol concentration, reflux time and solvent volume fold. The evaluating indicator was the extraction rate of total flavonoids from Tagetes erecta. The central composite design-response surface methodology was used to optimize the process and the prediction was carried out. RESULTS: The optimum conditions of extraction were 80% ethanol, 2.5 hours for reflux, 35 volume folds of solvent and 70 degrees C. CONCLUSION: It shows that the optimum model is simple and highly predictive.
