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Master's Dissertation
DOI
https://doi.org/10.11606/D.3.2020.tde-20052021-110639
Document
Author
Full name
Mateus de Souza Buriti
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
São Paulo, 2020
Supervisor
Committee
Romero, Luis Alberto Follegatti (President)
Ferreira, Mathilde Julienne Gisele Champeau
Veggi, Priscilla Carvalho
Title in Portuguese
Extração de compostos bioativos da carnaúba (Copernicia prunifera) através de CO2 supercrítico.
Keywords in Portuguese
Ácidos
Carnaúba
Compostos fenólicos
Fluidos supercríticos
Abstract in Portuguese
A carnaubeira (Copernicia prunifera (Mill.) H.E. Moore) é uma planta nativa do nordeste brasileiro, usualmente encontrada em solos salinos e inundáveis, com grande importância econômica na região promovendo também a preservação do bioma nativo e a mitigação da pobreza no campo. Extratos da semente e casca foram obtidos por extração Soxhlet sendo caracterizados em seguida por cromatografia de camada delgada (CCD) afim de identificar as possíveis classes de metabólitos secundários presentes. Compostos com atividade antioxidante foram identificados em todas as amostras de frações do fruto, especialmente para as extrações alcóolicas da semente onde foram identificados taninos. A extração supercrítica com dióxido de carbono (SC-CO2) foi empregada, como alternativa aos métodos convencionais de extração, para extrair compostos bioativos do fruto da carnaubeira. Os efeitos da pressão (200 e 300 bar) e da temperatura (40 e 80 ºC) sobre o rendimento global foram investigados com diâmetro de partícula médio (1,54 mm), vazão de CO2 (2,5 x 10-4kg/s) e uma razão entre massa de solvente e massa de matéria-prima (S/F = 54) mantidos constantes inicialmente. Posteriormente, usou-se a melhor condição de pressão e temperatura (300 bar/80 ºC) para avaliar efeito de diferentes razões S/F (36 e 72) e em menor diâmetro de partícula médio (0,77 mm) no rendimento global. O maior rendimento de óleo da semente de carnaúba (6,16%) correspondente a 68% em relação à extração Soxhlet foi obtido com S/F de 54, a 80 ºC e 300 bar e 0,77 mm de diâmetro médio. Uma avaliação sobre a extração com CO2 supercrítico foi realizado à casca da carnaúba estudando os efeitos da pressão (100, 200 e 300 bar), temperatura (40, 60 e 80 ºC) e vazão de etanol como cossolvente (0, 0,8 e 1,7 mL/min). O diâmetro geométrico médio igual a 0,49 mm, vazão de CO2 de 2,5 x 10-4kg/s e uma razão S/F de 30 foram mantidos constantes. Os resultados mostraram que o parâmetro de maior influência no rendimento global foi o uso de cossolvente que aumentou o rendimento para 13,29 quando a 100 bar, 80 ºC e 1,7 mL/min de vazão de etanol. Finalmente, os extratos da semente obtidos foram investigados em termos de perfil de ácidos graxos e da quantidade de compostos bioativos. O perfil de ácidos graxos de média cadeira (AGMC) foi melhor quando o maior diâmetro médio de partícula, S/F de 54, 80 ºC e 200 bar foram usados. Enquanto, a quantidade de tocóis foi máxima (354,94 mg/Kg de sementes) em S/F de 54, a 80 ºC, 300 bar e 1,54 mm e o ?-tocoferol foi o isômero em maior quantidade (269,77 mg/Kg de sementes). O ?-tocoferol foi encontrada predominantemente nas extrações Soxhlet. O método de atividade antioxidante (DPPH) foi realizado para os extratos alcóolicos da semente e casca obtidas na etapa de caracterização por CCD e da casca por fluido supercrítico. Encontrou-se grande potencial no extrato Soxhlet da semente utilizando álcool com IC50 de 82,76 µg/mL. Por outro lado, a fração alcóolica da casca extraída por Soxhlet e pelos ensaios preliminares de extração supercrítica da casca não demonstraram capacidade inibitória de radicais livres nas concentrações estudadas.
Title in English
Extraction of bioactive compounds from carnauba (Copernicia prunifera) using supercritical CO2.
Keywords in English
Carnauba (Copernicia prunifera)
Lauric acid, Tocols
Phenolic compounds
Supercritical fluid extraction
Abstract in English
The carnauba tree (Copernicia prunifera (Mill.) H.E. Moore) is a plant native to northeast region of Brazil which is usually found in saline and poorly drained soils. Its exploitation and extractivism has great economic importance for the region providing also the preservation of the native biome and the mitigation of poverty in the countryside. The extracts of the skin and seeds were obtained by Soxhlet extraction and then characterized by thin layer chromatography (TLC) in order to identify the classes of secondary metabolites. The technique identified the presence of compounds with antioxidant activity in all samples of fractions of the fruit, especially for the alcoholic extractions of the seeds where tannins were identified. Thus, supercritical extraction with carbon dioxide (SC-CO2) was used, as an alternative method, to extract bioactive compounds from the fruit. The effects of pressure (200 and 300 bar) and temperature (40 and 80 ºC) on global yield were investigated with average particle diameter (1.54 mm), CO2 flow (2.5 x 10-4 kg/s) and a ration between mass of solvent and mass of raw material (S/F = 54) kept constant initially. Subsequently, the best pressure and temperature condition (300 bar/80 ºC) was used to study the effect of different S/F rations (36 and 72) and a smaller average particle diameter (0.77 mm) on the global yield. The highest global yield of carnauba seed oil was obtained with S/F equal to 54, at 80 ºC and 300 bar when the particle diameter was the smallest one. The oil recovery, in those conditions, in comparison to Soxhlet extraction was 68%. An evaluation on extraction by supercritical CO2 was carried out on the carnauba fruit skin studying the effects of pressure (100, 200 and 300 bar), temperature (40, 60, 80 ºC) and ethanol co-solvent flow rate (0, 0.8 and 1.7 mL/min). An average geometric diameter of 0.49 mm, CO2 flow rate of 2.5 x 10-4 kg/s and an S/F ration of 30 were kept constant. The results showed that the parameter with the greatest influence on global yield was the use of co-solvent increasing the yield to 13,29% at 100 bar, 80 ºC and 1,7mL/min flow rate of ethanol. Finally, the obtained extracts were investigated in terms of fatty acid profile and quantity of bioactive compounds. The medium chain fatty acid profile was the highest in the largest mean particle diameter, S/F equal to 54, 80 ºC and 200 bar. Meanwhile, tocols content was maximum when S/F was held at 54, at 80 ºC and 300 bar when particle size was bigger (354.94 mg/Kg seeds) and ?-tocopherol was the most present isomer (269.77 mg/Kg seeds). ?-tocopherol content was found richer in Soxhlet extractions. The antioxidant activity method (DPPH) was performed for the alcoholic extracts of seed and fruit skin obtained in CCD step and for fruit skin obtained by supercritical extraction. Great antioxidant potential was found in the Soxhlet extract of the seed using ethanol with an IC50 of 82,76 µg/mL. On the other hand, the alcoholic fraction of the fruit skin extracted by Soxhlet and in the preliminary assays of supercritical extraction of the fruit skin did not demonstrate inhibitory capacity of free radicals in the studied concentrations.
 
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Publishing Date
2021-05-20
 
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