Design and Evaluation of Processes to Obtain Antioxidant-Rich Extracts from tropical fruits ...

247 Pages·2014·4.28 MB·English

Design and Evaluation of Processes
to Obtain Antioxidant-Rich Extracts
from tropical fruits cultivated in
Amazon, Caldas and Northern Tolima
Regions

Ivonne Ximena Cerón Salazar

Universidad Nacional de Colombia Sede Manizales
Facultad de Ingeniería y Arquitectura, Departamento de Ingeniería, Electrónica y
Computación
Manizales, Colombia
2013
II Design and Evaluation of Processes to Obtain Antioxidant-Rich Extracts from tropical
fruits cultivated in Amazon, Caldas and Northern Tolima Regions
Design and Evaluation of Processes
to Obtain Antioxidant-Rich Extracts
from tropical fruits cultivated in
Amazon, Caldas and Northern Tolima
Regions

Ivonne Ximena Cerón Salazar

Thesis submitted in partial fulfilment of the requirements for the degree of:
Doctor of Philosophy in Engineering

Advisor:
Carlos Ariel Cardona Alzate, Ph. D.
Co-advisor:
Juan Carlos Higuita Vásquez, Ph.D.

Research line:
Chemical and Biotechnological Processes Engineering
Research group: Chemical, Catalytic and Biotechnological Processes

Universidad Nacional de Colombia Sede Manizales
Facultad de Ingeniería y Arquitectura, Departamento de Ingeniería Eléctrica, Electrónica y
Computación
Manizales, Colombia
2013

VI Design and Evaluation of Processes to Obtain Antioxidant-Rich Extracts from tropical
fruits cultivated in Amazon, Caldas and Northern Tolima Regions

A Dios y la Virgen María. A mis madres Lucia
y Olga. A Franco, Jenny y Felipe.
VII

Acknowledgment

I would like to thank all the people who contributed in some way to the work described in
this thesis. First and foremost, I thank to my academic advisor and friend, Dr. Carlos Ariel
Cardona Alzate, for being an outstanding advisor and excellent professor. During my
studies, he contributed to me an enriching graduate school experience by giving me
intellectual freedom in my work, supporting my attendance at various conferences,
engaging me in new ideas, and demanding a high quality of work in all my endeavors. I
would like to express my deep gratitude and respect to Dr. Juan Carlos Higuita whose
advices and insight was invaluable for me and for all I learned from him. Thanks to all the
people who contributed with thesis with a discussion, an idea, information or guiding me in
confuse moments. To my research fellows and friends: Mauricio Naranjo, Jonathan
Moncada, Luis Eduardo Rincon, Julian Quintero, Alexander Posada, Valentina Hernandez,
Juan Jacobo Jaramillo, Monica Valencia, Javier Davila, Angela Idarraga, Sergio Duque,
Angela Gonzalez and Paola Moreno.

Thanks to the Universidad Nacional de Colombia for the financial support, to the Research
Office of National University of Colombia at Manizales for the financial support in this thesis,
projects and the internship in United States and Hungary, to the Faculty of Engineering and
Architecture of Universidad Nacional de Colombia at Manizales for the financial support in
air tickets, to the Department of Electricity, Electronic and Computational Engineering of
Universidad Nacional de Colombia at Manizales for the financial support for attending to
congresses. Kindly thanks to the Univesidad Nacional de Colombia to Amazonian for
financial support of projects and provide some fruits as raw materials.

I would like thank to Dr. Mahmoud El-Halwagi for receiving me at his laboratory during my
internship in the Texas A&M University, to Dr. Mario Eden for support during my visit to
Auburn University. I also want to thank to Dr. Barta Zsolt for the hospitality and help during
my internship in Hungary.

I would like to thank my family, especially my mother: Lucia, grandparents: Franco and Olga
for always believing in me, for their continuous love and their supports in my decisions.
Without whom I could not have made it here.
VIII Design and Evaluation of Processes to Obtain Antioxidant-Rich Extracts from
tropical fruits cultivated in Amazon, Caldas and Northern Tolima Regions

Abstract

In this thesis, a process design to obtain antioxidant-rich extracts from five tropical fruits
(i.e. Matisia cordata, Physalis peruviana, Solanum betaceum, Theobroma grandiflorum,
Renealmia alpinia) is presented. Simulation procedures based on experimental
characterization were used to evaluate the yield of different technologies for pretreatment,
extraction and concentration procedures using the Aspen Plus software. Both the
conventional and freeze drying technologies were evaluated as pretreatment methods
whereas conventional solvent and supercritical fluids were used for the extraction
procedure. The concentration stage was performed by using vacuum distillation or
ultrafiltration processes. Eight possible process configurations with mass integration were
evaluated with and without energetic integration in technical, economic and environmental
terms for each fruit. In this study, thermodynamic models were used in order to provide
convenient use of the operation conditions for all the technologies, this methodology permit
minimize the high costs and time that involve the experiments. The technical evaluations
presented in this work provide the feasibility of process configurations, which included the
evaluation of economic and environmental impacts. Nonetheless, several adjustments
must be done to implement this type of process at industrial scale, but this kind of analysis
serve as the basis draw recommendations for the efficient development processes. In this
work was also proposed several process configurations with both conventional and high-
end technologies for pretreatment, extraction and concentration stages. The major
disadvantage associate with the conventional technologies is the degradation of antioxidant
compounds by the possibility of oxidation of antioxidant compounds while the high-end
technologies retain the product quality. However, the major disadvantage of high-end
technologies is its relatively high cost. A common feature found in the process
configurations for all considered feedstock was the high influence of raw material costs in
total production cost. This work is a starting point to improve the tropical fruits productive
chain and integrate as possible new transformation alternatives. In order to compare the
simulation results, the polyphenolic compounds from each tropical fruit were extracted by
the different process configurations and the antioxidant activities of extracts were evaluated
with the purpose of compare the quality of the final product. Additionally, a process design
and an economic and environmental analysis for a biorefinery-based on an exotic fruit as
copoazu were performed. It was found that the uses of experimental data together with
simulation procedure are powerful tools for designing and analyzing the processes for
antioxidant rich-extracts. As final results it was demonstrated the feasibility of antioxidant
extraction for all fruits studied excepting the copoazu fruit. Additionally, it is important to
note that the R. alpinia peel contained relatively the highest amounts of polyphenolic
compounds with highest antioxidant activity. Finally, the antioxidant rich-extracts production
from tropical fruits could be considered as an opportunity to promote rural development with
the participation of small scale producers as feedstock suppliers.
Keywords: Process design; antioxidant; tropical fruits; polyphenolic compounds
Contenido IX

Resumen

En esta tesis se presenta un análisis del diseño del proceso para la obtención de extractos
ricos en antioxidantes a partir de cinco frutas trópicales (Cordata matisia, Physalis
peruviana, Solanum betaceum, Theobroma grandiflorum, Renealmia alpinia). Se utilizaron
procedimientos de simulación basado en la caracterización experimental para evaluar el
rendimiento de las diferentes tecnologías para las etapas de pretratamiento, extracción y
concentración utilizando el software Aspen Plus. Se utilizaron dos tecnologías para el
pretratamiento: secado convencional y secado por liofilización; para la extracción se
evaluarón extracción supercrítica y con solventes, mientras que para la etapa de
concentración se utilizó destilación al vacío y procesos de separación por membranas
“ultrafiltración”. Teniendo en cuenta lo anterior, ocho posibles configuraciones de proceso
con integración masica fueron evaluadas con y sin integración energética en términos
técnicos, económicos y ambientales de cada fruta. Además, se utilizaron modelos
termodinámicos para determinar las condiciones de operación para todas las tecnologías,
esto permitió minimizar los altos costos y el tiempo que implican los experimentos. Las
evaluaciones técnicas que se presentan, incluyen la evaluación de los impactos
económicos y ambientales. No obstante, estudios posteriores son necesarios para poner
en práctica este tipo de proceso a escala industrial, pero este tipo de análisis sirven como
base para el desarrollo de procesos eficientes. La principal desventaja asociada con las
tecnologías convencionales es la degradación de los compuestos antioxidantes dado a la
oxidación de compuestos antioxidantes, mientras que las tecnologías de gama alta
conservan la calidad del producto, sin embargo, su costo es relativamente alto. Una
característica común en las configuraciones de proceso fue la gran influencia de los costos
de las materias primas en el coste de producción total. Este trabajo es un punto de partida
para mejorar la cadena productiva de frutas tropicales e integrar como posibles nuevas
alternativas de transformación. Con el fin de comparar los resultados obtenidos por
simulación, los compuestos polifenólicos de cada fruta tropical fueron extraídos por las
diferentes configuraciones de proceso y se evaluaron la actividad antioxidante de cada
extracto con el propósito de comparar la calidad del producto final. Además, se diseño una
biorefineria a base de copoazu a la cual se le realizó un análisis económico y ambiental.
Se encontró que el uso de los datos experimentales, junto con el procedimiento de
simulación son herramientas poderosas para el diseño y análisis de los procesos de
extracción de antioxidantes. Como resultado final se demostró la viabilidad de la extracción
de antioxidante para todas las frutas estudiadas con excepción de la fruta copoazú.
Además, es importante tener en cuenta que la cáscara de Alpinia R. contiene relativamente
cantidades más altas de compuestos polifenólicos con mayor actividad antioxidante. Por
último, la producción de extractos ricos en antioxidantes a partir de frutas tropicales podría
ser considerada como una oportunidad para promover el desarrollo rural con la
participación de los productores en pequeña escala, como proveedores de materia prima.
Palabras clave: Diseño de procesos; antioxidantes; frutas tropicales; compuestos
fenólicos.
X Design and Evaluation of Processes to Obtain Antioxidant-Rich Extracts from
tropical fruits cultivated in Amazon, Caldas and Northern Tolima Regions