Advances in Science, Biotechnology and Safety of Foods
Edited by
Santos García Hugo Sergio García Galindo Guadalupe Virginia Nevárez-Moorillón
Asociación Mexicana de Ciencias de los Alimentos, A.C.
An official publication of the Asociaci贸n Mexicana de Ciencias de los Alimentos, A.C. (AMECA)
ISBN: 978-607-95455-4-3 Published by the Asociaci贸n Mexicana de Ciencia de los Alimentos, A.C. First Edition
All Rights Reserved 漏2015 Asociaci贸n Mexicana de Ciencia de los Alimentos, A.C. No part of the material protected by this copyright notice may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying or recording of by any information storage and retrieval systems, without written permission of the copyright owner. Printed in Mexico
Contents Foreword……………………………………………………………………………….. Preface………………………………………………………………………………...... Editors………………………………………………………………………………...... Part I Food Chemistry and Biochemistry The Wild Mexican Blackberries: Plants for Antioxidant and Human Food………....... M.B. Silva-Adame, A.T. Chávez-Bárcenas, A.E. Bárcenas-Ortega, E.F. Hernández-Valdés, R.E. Pérez-Sánchez, P.A. García-Saucedo Extraction and Characterization of Dyes from Bouganvillea glabra for Potential Use as a Food Additive…………………………………………………………………… A. Osorio-Alva, D.I. Murillo-Monroy, F. Cruz-Sosa, L. Buendía-González, J. Orozco-Villafuerte Antioxidant Properties and the Potential Hypoglycemic Effect of Lambrisco (Vauquelinia corymbosa) Leaf Extracts Obtained Under Different Solid-Liquid Extraction Conditions …………………………………………………………………. K. Rojero, E. Joya, E. Ortega-Rivas, D. Morales-Corral, S.B. Pérez-Vega, I. Salmerón Stability and Antioxidant Activity of Seed-Coat Black Beans (Phaseolus vulgaris L.) Microencapsulated by Spray Drying …………………………………………………… I.M. García-Sánchez, S.L. Martínez-Vargas, A.A. Sánchez-Colín, P.V. Martínez-Reyes, A.Y. Guadarrama-Lezama, H. Carrillo-Navas, C. Pérez-Alonso Alternative Conditions for Polyphenolics Extraction from Black Common Bean (Phaseolus vulgaris L.) Varieties …………………………………………………...... S. G. Alba-Murguia, X. Aparicio-Fernández Evaluation of Antinutritional Factor Phytic Acid on Triticale AN66 from Coahuila State (Mexico), at Different Phenological State……………………………………….... A. A. Neira Vielma, E. Nava Reyna, A. Iliná, A.J. Lozano del Rio, G. Michelena, L.G. Gaona, J.L. Martínez Hernández Protein Hydrolysates Obtained from Azufrado (sulphur yellow) Beans (Phaseolus vulgaris): ACE-Inhibitory and Antioxidative Characterization………..………………. C.I. Fuentes-Gutiérrez, L.J. Germán-Báez, R. Gutiérrez-Dorado, S. Medina-Godoy, A. Valdez-Ortiz Shelf Life of Cookies with Flour Lentil and Microcapsules of Flaxseed Oil as a Source of Polyunsaturated Fatty Acids………………..……………………………………...... J.G. Báez González, M.P. Morones Ramírez, M G Alanís Guzmán, C.T. Gallardo Rivera, M.G. Ibarra Robles, M. E. Rodríguez Huezo Free Gluten Bakery Product for Celiacs ……………………………………………...... E. Ochoa-Reyes, H. De la Garza-Toledo, X. RuelasChacón, J.F. Hernández-Ángel, C.N. Aguilar, J. de J. Ornelas-Paz Dietary Fiber- Invertase Supplement for Sucrose Intolerance Regulation…………… C. Balvantín-García, E. P. Segura-Ceniceros, J. L. Martínez-Hernández, A. Ilina Mitigating effect of calcium and magnesium on acrylamide formation in tortilla chips..
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R. Salazar, G. Arámbula-Villa, E. Gutierrez-Arias, G. Luna-Bárcenas, E. Azuara Hybrids Development of Quality Protein Maize for Highlands Valleys of Mexico: Genetic Advance in Relation to Parents Average …………………………………...... 91 G. F. Gutiérrez-Hernández, J. L. Arellano-Vázquez, J. M. Vázquez-Ramos, E. García-Ramírez, P. Vázquez-Lozano Exploration of Aroma Quality of Mezcal by Sensory Analysis and Chromatographic Analysis………………………………………………………………………………...... 97 S. E. García-Barrón, A. Gschaedler-Mathis, H. B. Escalona-Buendía, S.J. Villanueva-Rodríguez Evaluation of the Acceptance of Mixed Stabilizers in Goat Milk Ice Cream ……………… 105 L. Hernández-González, L. Isidro-Requejo, S. Fernández-Michel, M.L. Froto-Madariaga Sensory Evaluation of Marinated Beef with Chía-Base Marinator …………………...... 111 S.M. Sánchez-Chi, J.A. Vázquez-Rodríguez, A.R García-Arellano, J.G. Báez-González, M.A. Núñez-González, C.A. Amaya-Guerra
Part II Food Biotechnology Effect of Fermentation Conditions on the Production of a Pineapple Wine (Ananas comosus (L.) Merrill) …………………………………………………………..………. M. Martínez-Minaya, E. N. Aquino-Bolaños, M. López del Castillo-Lozano Sensory Evaluation of Handcrafted Corn Malt Beverages: Sendechó and Corn Beer…. M.A Romero-Medina, N.N. Cruz-Rodríguez, H.B. Escalona-Buendía, J. R Verde-Calvo Production and Partial Characterization of Lipase from Aspergillus niger Obtained by Submerged Fermentation in Conventional Media ………………………………….…. D. Y. López, Y. Osuna, A. Iliná and J.L Martínez Preliminary culture conditions for carotenoids production by Rhodotorula glutinis YB-252 in solid-state fermentation ……………………………….…………………... A.Y. Hernández-Almanza, C.G. Martínez-Ávila, J.C. Montañez-Sáenz, R. Rodríguez-Herrera, C.N. Aguilar Pectin Oligomers Obtained By Enzymatic Hydrolysis of Guava And Papaya Cell Walls ……………………………………………………………………...……………. R. Vélez-de la Rocha, R. C. Heras-Gaspar, R, J.C. Contreras-Esquivel, J. A. Sañudo- Barajas Enzymatic Activity Of Peroxidase and Catalase from Fresh Coriandrum sativum and Petroselinum crispum ………………………………………………………………… A.M. García-Frayre, Y.T. Gallardo-Navarro, M.T. Cruz-y-Victoria.
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Part III Food Processing and Engineering Use of maguey (Agave spp.) leaves as a source of functional ingredients in cooked sausages elaboration ………………………………………………….………………... 163 B.I. Castillejos-Gómez, A. Totosaus, M.L. Pérez-Chabela iv
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Glass Transition and Water Activity of Model Food Systems Analogous to Fruit Powder Composition………………………………………………………………. M. Z. Saavedra-Leos, A. Grajales-Lagunes, R. González-García, A. Toxqui-Terán, S. A. Pérez-García, M. Abud-Archila, M. Moscosa-Santillán and M. A. RuizCabrera Thermal Analysis Characterization in Apple Osmotic Dehydration…………………. M. E. Rosas-Mendoza, J. L. Arjona-Román Mass Transfer Modeling during Osmotic Dehydration of Foods Shaped as Annular Cylinders ……………………………………………………………..………………... B. Ortiz-García-Carrasco, H. Ruiz-Espinosa, M.A. García-Alvarado, I.I. Ruiz-López Modeling the Apparent Density and Shrinkage Characteristics of Fruits and Vegetables during Convective Drying ………………………………..………………. E. Molinos-Badillo, H. Ruiz-Espinosa, M.L. Luna-Guevara, I.I. Ruiz-López Water Diffusivity Determination During Osmotic Dehydration of Kiwi Fruit and Guava Chips………………………………..…………………………………………... W.N. Hernández-Díaz, F.J. Hernández-Campos, C. Gomez-Cruz, J.A. Tinoco-Alonso, O. Quiroz-Cardoso,L.A. Arau-Roffiel, M.A. Benitez. Water Adsorption Isotherms for Tascalate, A Powder Employed To Make A Traditional Beverage Of Chiapas, México …………………………...………………... L.J. Corzo-Rios, M. A. Aguilar-Méndez, M.E. Ramirez-Ortíz Ratio of the Activation Energy of the Drying Process of Aqueous Solutions of Biopolymers With the Efficiency of Microencapsulation …………………………… J.G. Báez González, C.A. Amaya Guerra; M.A. Núñez González, M.E. Rodríguez Huezo, C.T. Gallardo Rivera, E.J. Vernon Carter Physical and rheological characterization of edible coatings formulated with a BWP (biopolymer - wax - polyol) system …………………………………………………… E. Ochoa Reyes, D.G. Martínez Vázquez, E. Jimenez Regalado, H. De La Garza Toledo, J.C. Montanez, R. Rojas, J. de J. Ornelas-Paz, C.N. Aguilar Production of Nixtamalyzed Corn Flour by Continuous Ohmic Heating……………… I. Ménera-López, M. Gaytán-Martínez, M.L. Reyes-Vega, E. Morales-Sánchez Optimization Osmotic Dehydration by Vacuum Packaging of Fresh-cut Mango.…… M.L. Zambrano-Zaragoza, A. Álvarez-Cárdenas, M.E. Jiménez-Vieyra, E. Gutiérrez-Cortez, G.G. Ayala Scale-Up and Sustainability Evaluation in the Solvent Extraction of Peanut Skin Antioxidants ……………………………………………………………………………………………………………… S.A. Medina-González, H.F. Almeida-Trasviña, I. Salmerón-Ochoa, D. Morales-Corral, S.B. Pérez-Vega Shelf Life Estimation of Extruded Snacks Expanded by Frying and by Using Hot Air Stored in Polypropylene and Metallized Polypropylene Packaging ………...………… J.C.I. Barcenas Serrano, J.G. Pérez Flores, A. Castañeda Ovando, J. Jaimez Ordaz, E. Contreras López Rehydration of Cooked-Lyophilized longissimus dorsi Pork…………..……………… J. Coria-Hernández, R. Meléndez-Pérez, J.L. Arjona-Román, J. López-Pérez, A. Llorente-Bousquets Effect of Heat Treatment on the Degradation of β-Carotene Nanocapsules in a
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Scraped Surface Heat Exchanger (SSHE)……………………………………………… R.M. González-Reza, M.L. Zambrano-Zaragoza, J.J. Flores-Minutti, D. Quintanar-Guerrero Precooling by Nanocapsule Coating Application and Hydrofluidization on Fresh-Cut Fruit……………………………………………………………………..……………… A. Álvarez-Cárdenas, J. Hernández-Viveros, T.L. Vázquez-Avila, D. Quintanar-Guerrero, M.L. Zambrano-Zaragoza A Feasibility Study for the Production of Added Value Compounds from Apple Waste: A Simulation Case……………………………………………………………… H.F. Almeida-Trasviña, S.A. Medina-González, E. Ortega-Rivas, S.B. Pérez-Vega Elaboration of a Carboxymethylcellulose/Gelatin Based Edible Coating for Application in Minimally Processed Golden Delicious Apple and Cantaloupe Melon... A.L. Velázquez Mendoza, J. Castillón Jardón
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Part IV Food Safety and Food Microbiology Pycnoporus sanguineus Pigment Extracts Against Phytopathogenic Fungi (Colletotrichum fragariae, C. gloeosporioides and Botrytis cinerea) ……………….... R. Cruz-Muñoz,, Y. M. Gómez-Gómez, G. Valencia-del-Toro, F. Robles-Martínez, J. Yañez-Fernández, R. Villanueva-Arce, S. Bautista-Baños Production of Pectate Lyase by Colletotrichum spp. from Mango Ataulfo as a Mechanism of Pathogenicity…………………………………………………………… A. Berecochea-López, J.A. Ragazzo-Sánchez, R. Allende-Molar, G.D. Avila-Quezada, H. Cabanillas-Beltrán, M. Calderon-Santoyo Evaluation Effectiveness Evaluation Of Extracts Of Wild And Cultivated Axihuitl (Eupatorium Aschembornianum Sch) To Control Phytopathogens …………………. J. Canales-Enriquez, E. Nava-Reyna, G. Rincón-Enriquez, A. Iliná, J.L. Martínez-Hernández Plant Growth Promoting Bacteria in the Nutraceutical Quality of Mexican Strawberry Fruits……………………………………………………….…………………………... M.A. González-Urías, G. Vázquez-Gálvez, J. Molina-Torres, E. Ramírez-Chávez, L.F Soria-Martínez, R. Serrato-Flores, M.V. Angoa-Pérez, H.G Mena-Violante Analysis of Some Mechanisms of Inhibition by Chitosan in Cell Germination of Colletotrichum sp. Isolated from Banana Fruits (Musa sapientum).………………….... V.A. Ochoa-Jiménez, G. Berumen-Varela, M.A. Chacón-López, P. Gutiérrez-Martínez Isolation and Molecular Identification of Curvularia lunata/Cochliobolus lunatus Causal Agent of Leaf Spot Disease of Cocoa …………………………………..…...... J. A. Cuervo-Parra, T. Romero-Cortes, M. Ramírez-Lepe Antimicrobial Activity of Rosmarinus officinalis on Methicillin-Resistant Staphylococcus aureus, susceptible Staphylococcus aureus and Salmonella typhi. ………
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Antimicrobial Activity Against Escherichia coli or Listeria monocytogenes of Extracts Obtained from Three Mexican Pepper (Capsicum) ………………………… T.G. Cerón-Carrillo, N.A. Santiesteban-López, A. López-Malo, E. Palou Viability of Lactobacillus paracasei Encapsulated by Spray Gun…………………… A.G. Peredo Lovillo, H.E. Romero Luna, C.I. Beristain Guevara, E. Azuara Nieto, G. Luna Solano, M. Jiménez Fernández Use of ICMSF sampling programs for the detection of Listeria spp in pork obtained from a TIF slaughterhouse……..……………………………………………………… S. García-Pedraza, J. López-Pérez, A. Llorente-Bousquets
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Foreword When we talk about science, biotechnology and safety of food, we encompass critical areas, not only for the survival of the population, but also to provide ways to improve the wellbeing of society. Every region, country or consortium of countries, must work in these areas to improve or maintain the quality of food provided for their own people. Academia, government and industry also must work together to promote food security, safety, quality and innovation. Working together is the key, and this team has the tools to discover, develop or innovate in the science of food and apply these results to resolve challenges facing our society. The studies presented in this book reflect the effort of many institutions to provide better food. Many of them reflect the cooperation between national institutions, which is needed in most cases to generate more information. Others show international collaborative efforts most of them to resolve international or global challenges. The main objective of this book is to publish selected studies presented at the 5th Food Science and Food Biotechnology in Developing Countries. These studies provide an idea of what is being done in our societies. What needs to be clarified is that this kind of science is not “developing science” conducted in developing countries, but modern science conducted in developing countries to be applied globally. As seen in this book, traditions and behaviors are unique to specific regions or countries. Each of the latter, are able to provide much information and many resources to develop, innovate and offer an unlimited number of food products to the word. On the other hand, the unlimited possibilities for the mixing compounds and use of various technologies to grow, produce and process foods, are what make food science very attractive to me and to others.
Dr. Santos García President, Asociación Mexicana de Ciencias de los Alimentos
Preface The book constitutes a volume, part of a series, based on selected contributions presented at the 5th International Congress on Food Science and Food Biotechnology in Developing Countries. The congress took place at Nuevo Vallarta, Nayarit, Mexico, in October 2012. The event gathered experts and delegates, not only from developing countries but from nations all around the globe, and served the purpose of discussing and analysing the stateof-the-art on food science, food biotechnology and Food Safety. The main objective of the series of congresses organised by AMECA has been always to promote a harmonic development in research and technology transfer in the ample subject of food science and food biotechnology. The strategy has been aimed at placing into perspective the situation of research efforts of developing countries but with the intention to promote exchange, discussion, and analysis with the global academic community, in order to seek a more uniform development in the general area of food sciences. So far the series of congresses have provided a proper forum of interaction of all the sectors involved in food production, processing and distribution, including students, academics, and industrialists alike. The book comprises four sections or parts, dealing with relevant main themes of the subject of food science, i.e.: food chemistry and biochemistry, food biotechnology, food processing and engineering, and food safety and microbiology. Food chemistry and biochemistry section includes topics of food properties, nutrition, functional foods, sensory evaluation, etc. Food biotechnology focuses on topics like food fermentations, enzymes in foods, etc. Food processing and engineering includes conventional processing and preservation technologies, such as drying and pasteurisation, as well as non-predominant food methodologies including ohmic heating. Each part includes several research papers drawn from the voluntary contributions of the meeting. The purpose of the book is to give an insight on how food components and preservation technologies can be combined to provide healthy foods to the world population.
Santos García Hugo Sergio García Galindo Guadalupe Virginia Nevárez-Moorillón
Chapter 36
Effect of Heat Treatment on the Degradation of βCarotene Nanocapsules in a Scraped Surface Heat Exchanger (SSHE) González-Reza R.M.a,b, Zambrano-Zaragoza M.L.b*, Flores-Minutti J.J.a and Quintanar-Guerrero D.c a
Facultad de Estudios Superiores Cuautitlán, Universidad Nacional Autónoma de México, Departamento de Ingeniería y Tecnología, Laboratorio Experimental Multidisciplinario LEM-A Av. 1o de mayo s/n Cuautitlán Izcalli C.P. 54745, Edo, de México, México. b Facultad de Estudios Superiores Cuautitlán, Universidad Nacional Autónoma de México, Laboratorio de Procesos de Transformación y Tecnologías Emergentes en Alimentos. Km 2.5 Carretera Cuautitlán–Teoloyucan, San Sebastián Xhala, Cuautitlán Izcalli, Edo de México, CP.54714, México. c Facultad de Estudios Superiores Cuautitlán, Universidad Nacional Autónoma de México, Laboratorio de Posgrado en Tecnología Farmacéutica, Av. 1 o de mayo s/n Cuautitlán Izcalli C.P. 54745, Edo, de México, México.
Abstract Response surface methodology (RSM) was used to optimize the conditions of the pasteurization process in thermal degradation of nanocapsules of β-carotene in a scraped surface heat exchanger (SSHE). The variables studied were pump speed (40-80 %), steam pressure (0.5-1.5 Bar) and rotor speed (100-300 rpm). The thermal degradation was evaluated by spectrophotometric measurements of the β-carotene at λ = 480 nm. Thermal degradation of nanocapsules was evaluated once the pasteurization process was optimized in function of thermal degradation of β- carotene into nanocapsules. Polymeric nanocapsules were obtained by the emulsification-diffusion method. Dispersion was evaluated by its particle size (PS), polydispersion index (PDI) and zeta potential (ζ). The scanning microscopy evaluation confirms the presence of capsular structures. Analyzed responses for nanocapsules resulted in total loss of β-carotene, as well as final content and changes in activation energy (Ea) during pasteurization. As it is common in food science, decimal reduction time (D) was evaluated using non-encapsulated β-carotene since protection afforded by the polymer overestimated the values of this parameter and, thus, ensured pasteurization. Results showed that experimental data could be adequately explained for a second-order polynomial model with multiple regression coefficients [R2] of 0.97 - 0.99. Results also showed that the variable with the greatest significance in the indicator degradation were steam pressure and pump speed (p<0.0001). The optimal process conditions obtained for thermal degradation of nanocapsules of β - carotene were 82.8 % of pump speed, rotor speed of 283 rpm and steam pressure of 1.24 Bar, with optimum values of Ea = 140 kJ/mol, D = 5 min. with a maximum loss of encapsulated β-carotene=16%. It was concluded that the formation of nanocapsules provides an application in conservation of thermolabile compounds in a thermal process such as pasteurization, since it avoids any significant loss of β-carotene due to thermal resistance offered by forming the base capsular polymeric.
Keywords: Nanocapsules, β-carotene, thermal treatment, SSHE, thermal degradation
*
Corresponding author: Phone: +52(55)56231999 ext 39406, Email: luz.zambrano@unam.mx
Science, Biotechnology and Safety of Foods
Introduction Surface scraped heat exchangers (SSHE) are often used in the food industry to process highly viscous fluids. The main specificity of these exchangers lies on the rotation of a rotor equipped with floating blades which scrape periodically the exchange surface in order to prevent its clogging and to promote heat transfer. However, it appears that the thermal and mechanical treatment received by the viscous product is very different depending on the operating conditions as residence time distribution, viscosity, velocity, among others (Mabit et al., 2008). Specifically, scraped-surface heat exchangers (SSHE’s) are widely used in food industry to cook, chill, crystallize or sterilize certain foodstuffs quickly and efficiently without causing unwanted changes to the constitution, texture and appearance of the final product (Duffy et al., 2007). The molecule of β-carotene is an important member of the carotenoids family found in many fruits and vegetables. Besides its high provitamin A activity and antioxidant capacity, β-carotene possesses many health-benefiting effects, including protection against a number of serious health disorders, e.g. cancer, cardiovascular disease, macular degeneration. For these reasons, there is an increasing interest in incorporating β-carogene as functional ingredients in food formulations. However β-carotene is insoluble in water and only marginally soluble in oil at room temperature because of its crystalline form. This greatly limits the development of β-carotene enriched food products, and even decreases its bioavailability. Another limitation for β-carotene to be applied in food industry is that it is sensitive to light, oxygen, and even heat. One effective strategy to protect and deliver the sensitive ingredients is to microencapsulate them within a coating or wall material (Dutta et al., 2006; Inbara et al., 2008; Qiu et al., 2009; Deng et al., 2014). Emulsification–Diffusion Method (EDM) allows the preparation of nanocapsules (NCs) which structure enhances encapsulation of lipophilic active-substances. The method involves the formation of an oil-in-water emulsion formed by an oily phase of a partially water-miscible solvent (previously saturated) which contains a polymer and an oil and an aqueous phase (previously saturated) which contains a stabilizer. The dilution of this emulsion (diffusion process) triggers the aggregation of both oil and polymer in nanocapsules (Mora-Huertas et al., 2010). EDM is a good option to prepare harmless and safe food nanosystems, particularly biodegradable NCs, considering the low residual amounts of stabilizer and solvent after conventional purification (Quintanar-Guerrero et al., 1998; Zambrano-Zaragoza et al., 2011).
Materials and Methods Materials Poly-ε-caprolactone (PCL) (Mw ~80 kDa, ρ = 1.147 s/cm3 at 25°C) was obtained from Sigma-Aldrich® (USA). The stabilizing agent was Pluronic®, F-127 (Poloxamer 407, PF127) (BASF, México). Sunflower oil (ρ=0.921 g/cm3 at 25 °C), β-carotene was used as oily core from Sigma-Aldrich® (USA). The partially water-miscible solvent was ethyl acetate (EA) HPLC grade supplied by Fermont (México). This solvent was selected due to their low toxicity (ICH class: 3). Distilled water was of Milli-Q quality (Millipore®, USABedfore, MD). All other reagents were of analytical grade and were used without further purification. 262
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Nanocapsules Preparations NCs were produced by the Emulsification-Diffusion Method (EDM) described in detail elsewhere (Quintanar-Guerrero et al., 1998) according to optimization performance proposed by Zambrano-Zaragoza et al., (2011). Particle Size (PS) and Polydispersion Index (PDI) PS distribution and PDI were determined by laser light scattering technique at 273° fixed angle and 25ºC, using a Z-sizer 4 (Zetasizer Nano Series Malvern Ltd, France). Dispersion was diluted in Milli-Q® water, according to the volume frequency histogram. Measurements were made at 25°C in triplicate. Zeta Potential (ζ) ζ was evaluated for the system using a Z-sizer 4 (Zetasizer Nano Series, Malvern Ltd, France) after proper dilution in distiller water Milli-Q®. ζ values were normalized with polystyrene standard dispersion (ζ = -55 mV). Measurements were made at 25°C in triplicate. Morphological studies NCs were purified by three steps of ultracentrifugation (30,000 rpm for 30 min at 5°C) in order to eliminate the excess stabilizer. A droplet of this concentrated suspension was spread on a glass surface and dried. Finally, the dried sample was mounted on stubs and shadowed in a gold-layer cathodic evaporator(~ 20 nm) using a JFC-1100 Sputter Coater (JEOL, Tokyo, Japan), and was then observed under a low vacuum scanning electron microscope (LV-SEM, JSM 5600 LV) with a 5 nm resolution. NCs micrographs were obtained with equipment settings of 20kV electron acceleration voltages and a pressure of 12 - 20Pa in the specimen chamber. Residence Time Distribution (RTD) Fluid RTD within the SSHE was measured using a tracer response technique. The experiments were conducted with a fluid pulse injection of 1% of the dead volume in each section of the process (heating, heating + maintenance and total residence), a blue dye number 5 with a concentration of 300 μg/ml using a model fluid a dispersion of CMC 0.5 with NCs. Tracer was injected immediately before the SSHE inlet using a spring loaded piston which introduced the tracer. The light absorbance of the outlet stream was measured continuously at λ = 630 nm using a spectrophotometer (Cintra 10 UV – Visible, GBC Scientific Equipment, Australia). β-carotene Degradation Kinetic Modeling The residual β–carotene was determined by spectrophotometry (Cintra 10 UV-Visible) at λ=480 nm to the output of exchanger, all measurements were done in triplicate. β-carotene concentrations were obtained from a calibration curve. The kinetics of degradation of βcarotene was described by a kinetic first order reaction using the Arrhenius equation (Ea) in addition to decimal reduction time (D).
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Experimental Design The experimental design was a central composite routable design, with 8 factorials points, 6 central points and 6 axial points with α=1.68719. It was done in order to obtain the coefficients of the response surface equation. ANOVA analysis was done to evaluate any significant differences between the independent variables using MINITAB release 16 (Minitab Inc., PA, US).
Results and Discussion Particle size, PDI and zeta potential (ζ) Nanocapsules had an average particle size of 300 nm with a PDI of 0.16, indicating a submicronic size with narrow particle distribution. The ζ was of -36.45 mV suggesting a physical stable dispersion with low probability of aggregation (Schramm, 2006). Nanocapsules Morphology Figure 1 shows the micrographs corresponding to the nanocapsules of β-carotene. They are the best evidence the capsular structure consisting of an oily nanodroplet with surrounded by a thin envelope (Zambrano-Zaragoza et al., 2011).
Figure 1. Micrographs of nanocapsules of β-carotene.
Residence Time Distribution (RTD) Figure 2 shows the effect of flow rate (26 - 93 %) and the steam pressure (0.5 - 1.5bar) on residence time for determination of degradation rates in NCs according to the Arrhenius law. The distribution of residence times followed normal behavior. The greater influence was of flow velocity, reflected by the changes in the amplitude of the distribution which had the highest age distribution when the flow was of 26 %. The stream pressure has an effect on rheological properties that contribute to increased age frequency and the narrow
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distribution when steam pressure was of 1.5 bar minimized the resistance effect of rotor speed (Pinheiro Torres and Olivera, 1998). 1.6 1.4
93.6% 1Bar
1.2 80% 1.5Bar
E (θ)
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0.5
Tiempo (θ) Figure 2 Characterization of flow behavior with NCs of β-carotene dissolved in CMC 0.5
Analysis of response surfaces In order to visualize the effect of the independent variables on the dependent ones, surface response and contour plots of the quadric polynomial models were generated by varying two of the independent variables within the experimental range while holding the other constant at the high factorial points. a) Activation Energy (Ea). Figure 3a-b shows the response surface of the energy activation of NCs. Figure 3a reveals that there is a significant curvature around the central point of the model (R2=0.9925), being the most significant factors all linear terms and interactions (p<0.000) with a maximum Ea of 186.79 kJ/mol when rotor speed is 31.82 rpm and the steam pressure is around 1 bar. Figure 3b shows a similar behavior around the central points with a maximum of 175 kJ/mol. Equation (1) is the second order model for Ea (Y1) in significant terms: Â&#x192; ŕľ&#x152; ʹǤͺͳ ଵ ŕľ&#x2026; ͲǤʹʹ ଶ ŕľ&#x2026; ʹͲ͸Ǥʹ͜ ଷ ŕľ&#x2020; ͲǤͲʹ ଵଵ ŕľ&#x2020; ͸ͺǤ;ʹ ଷଷ ŕľ&#x2020; ͳǤͲ͸ ଵଷ ŕľ&#x2020; ͲǤͳ͚ ଶଷ (1)
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Rotor Speed (rpm)
Steam Pressure (Bar)
b)
Ea (kJ/mol)
a)
Figure 3. Response surface (a) and contour (b) plots of the activation energy as a function of (a) rotor speed and steam pressure (b) steam pressure and pump speed of 80% and 300 rpm, respectively.
b) Loss of Nanoencapsulated ﾎｲ窶田arotene. The maximum loss of ﾎｲ-carotene nanocapsules was at pump speed 60 %, rotor speed 200 rpm and steam pressure 1.84 bar with a value around 30%. The minimum loss was at pump speed 94.64 %, rotor speed 200 rpm and steam pressure 1 bar with a value of 7%. c) Decimal Reduction Time (D). The effects of the independent variables on decimal reduction time are shown in Figure 4a-b. Figure 4a was generated by varying the pump speed and rotor speed while holding steam pressure 1.5 bar and it shows the response surface of the independent variables being the most significant factors all linear terms and interactions (p<0.000) with a minimum D = 2.49 min (Van Boekel, 2009) when rotor speed is 200 rpm and the pump speed is 93.64%. Figure 4b was generated by varying the rotor speed and steam pressure while maintaining pump speed at 80 %. a)
Pump Speed (%)
Rotor Speed (%)
D (min)
b)
Figure 4. Response surface (a) and contour (b) plots of the decimal reduction time as a function of (a) pump speed and rotor speed (b) rotor speed and steam pressure of 1.5 bar and 80%, respectively.
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The expression evaluated for D (Y2) of unencapsulated β-carotene is: ŕľ&#x152; ͳ͜Ǥͺ͸ ŕľ&#x2020; ͳǤ͸ ିଷ ଵଵ ŕľ&#x2026; Íś ିସ ଵଶ ŕľ&#x2026; ;Ǥ͸; ିଶ ଵଷ ŕľ&#x2020; ʹǤʹ͡ ିଶ ଶଷ (2)
Optimization The optimal process conditions obtained for the thermal degradation of β-carotene nanocapsules were 82.8 % of pump speed, rotor speed of 283 rpm and steam pressure of 1.24 Bar, with optimum values of Ea = 140 kJ/mol, D = 5 min. with a maximum loss of βcarotene nanoencapsulated of 16%.
Conclusions The current study showed that the second-order polynomial model fits to describe and to predict the responses of the activation energy and loss of β-carotene nanocapsules. The independent parameters and the quadrics had a significant effect on the loss and activation energy of nanocapsules of β-carotene. Nanoencapsulation provides an additional protector effect that avoids the degradation of thermolabile compounds in a thermal process such as pasteurization; this effect is attributed to the presence of the membrane film formed around the oily core.
Acknowledgements The authors acknowledge the financial support for this work from PAPIIT: IT200814 and IT201914 of the DGAPA-UNAM. We would like to thanks M en I.Q. Alicia del Real for taking the micrographs of nanocapsules.
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