PROCESS OF EXTRACTION AND PURIFICATION OF CAFFEINE FROM PLANTS AND FRUITS BY USING HYBRID METHODOLOGIES

The present disclosure is related to the purification of caffeine from coffee husk using water, ethanol and a stripping resin. Water acts as an extracting agent and ethanol allows the recovery of bioactive compounds after performing a resin-filled column liquid chromatography. The process begins wit...

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Hauptverfasser: ASCACIO VALDES Juan Alberto, FLORES GALLEGOS Adriana Carolina, RODRÍGUEZ HERRERA Raúl, NERY FLORES Sendar Daniel, CRUZ REQUENA Marisol, DE LA PEÑA GONZALEZ Jonathan Emmanuel, SAENZ GALINDO Aide, PALOMO LIGAS Lissethe
Format: Patent
Sprache:eng ; spa
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Zusammenfassung:The present disclosure is related to the purification of caffeine from coffee husk using water, ethanol and a stripping resin. Water acts as an extracting agent and ethanol allows the recovery of bioactive compounds after performing a resin-filled column liquid chromatography. The process begins with the dehydration and grinding of the coffee husks at room temperature for a period of 10 days, then the extraction is carried out in a mass/volume ratio of 1:5 (1 part of dehydrated and ground material for 5 parts of water) at a temperature of 60°C for 30 minutes, the extract is filtered to obtain the aqueous part. A column is packed with the resin and unwanted compounds are removed. Subsequently, a second elution is carried out with ethanol to recover the fraction of bioactive compounds separated thanks to the interaction with the resin. Subsequently, the residual ethanol is evaporated at a temperature of 60°C to recover a fine powder. This obtained powder is purified by polarity separation using polar solvents (ethyl acetate, ethanol and methanol) and non-polar solvents (hexane and chloroform). To corroborate the separation of compounds, thin layer chromatography was performed with hexane as the mobile phase and characterized by FTIR spectroscopy. Finally, the polar extract was characterized by mass spectrometry and identified as caffeine. La presente describe la purificación de cafeína a partir de cáscara de café empleando agua, etanol y una resina de separación. El agua actúa como agente extractor y el etanol permite la recuperación de los compuestos bioactivos después de realizar una cromatografía de líquidos en columna rellena con resina. El proceso comienza con la deshidratación y molienda de las cáscaras de café a temperatura ambiente por un periodo de 10 días, posteriormente la extracción se lleva a cabo en una relación masa/volumen de 1:5 (1 parte de material deshidratado y molido por 5 partes de agua) a una temperatura de 60 °C por 30 minutos, el extracto es filtrado para obtener la parte acuosa. Se empaca una columna con la resina y se eliminan los compuestos no deseados. Posteriormente se realiza una segunda elución con etanol para recuperar la fracción de compuestos bioactivos separados gracias a la interacción con la resina. Posteriormente, el etanol residual es evaporado a una temperatura de 60 °C para recuperar un polvo fino. Este polvo obtenido es purificado mediante separación por polaridad utilizando solventes polares (acetato de etilo, etan