Development, evaluation and application of symbiotic microparticles produced by spray chilling technology

Foram produzidas micropartículas simbióticas com carreador de natureza lipídica, obtidas por spray chilling. Como materiais ativos foram utilizadas duas cepas de micro-organismos probióticos (L. acidophilus-LA e L. rhamnosus-LR), dois prebióticos (inulina e polidextrose) e gordura de palma e palmiste interesterificada. Estudou-se a resistência destes probióticos ao processo aplicado, o comportamento das micropartículas sólido lipídicas (MSLs) frente ao fluido gástrico e intestinal simulados e suas viabilidades durante 120 dias de armazenamento à -18, 7 e 22°C sob vácuo ou umidade relativa controlada. A caracterização morfológica, granulometria, análise térmica (DSC), atividade de água, espectroscopia na região do infravermelho (FTIR) e difração de raios-X (XRPD) foram estudados. Spray chilling configurou-se como processo adequado aos probióticos, devido à baixa perda de células viáveis durante a obtenção das micropartículas, sendo que não foi observado interferência da ausência, presença e do tipo de prebiótico. Foram obtidas MSLs esféricas com superfície relativamente uniforme, e com tamanho médio entre 62,4±2,8 a 69,6±5,1 µm, sendo que não houve diferença significativa entre as formulações. As análises de difração de raios-X indicaram que não ocorreram alterações polimórficas durante o armazenamento refrigerado das MSLs. Quanto à análise térmica pode-se dizer que a presença de probióticos e prebióticos praticamente não interferiu na alteração da temperatura de fusão para todas as formulações estudadas, que variou de 45,37°C a 47,58°C, inferindo-se a ausência de interações significativas entre os ingredientes microencapsulados e o carreador, ausência que foi reafirmada pelos espectros de infravermelho. A microencapsulação favoreceu a sobrevivência frente aos fluidos gástrico e intestinal simulados, e possibilitou a manutenção de células viáveis acima de 106 UFC por grama até 120 dias de armazenamento em umidade relativa controlada para a formulação com L. acidophilus e polidextrose, a qual foi influenciada pela atividade de água da partícula, que por sua vez foi afetada pela incorporação de prebióticos. Tendo em vista o potencial da MSLs desenvolvidas, estas foram incorporadas ao sorvete. Nesta matriz as micropartículas não apresentaram um bom desempenho, seja na sobrevivência de L. acidophilus durante o armazenamento do produto, como na proteção diante da exposição às condições gastrointestinais simuladas. Além disso, sorvetes com adição das MSLs foram avaliados com notas significativamente menores (p≤0,05) nos atributos textura, sabor e aceitação global em relação a amostras controle e a com adição de probióticos livres na análise sensorial do produto desenvolvido. As micropartículas lipídicas produzidas mostraram-se aptas como ingrediente alimentício, porém no sorvete não atenderam as premissas de proteção e extensão de contagens apropriadas do probiótico. As MSLs também foram incorporadas em polpas de fruta, abacate e melão, neste tipo de matriz as MSLs conferiram proteção ao micro-organismo pois aumentaram sua viabilidade em relação aos micro-organismos livres.Symbiotic microparticles were produced with a lipid carrier, obtained by spray chilling technology. In this study were used two strains of probiotic (L. acidophilus-LA and L. rhamnosus-LR) and two prebiotics (inulin and polydextrose) as active or core materials. The resistance of these probiotics to the spray chilling process was evaluated, as well as the viability of the solid lipid microparticles (SLMs) during the exposition to the simulated gastric and intestinal fluids and stability during 120 days of storage at -18, 7 and 22°C, in vacuum or controlled relative humidity. Morphology characterization, particle size, water activity, thermal analysis (DSC), infrared spectroscopy and X-ray diffraction (XRPD) were studied. Spray chilling process was configured as a suitable technology to probiotics due to low loss of viable cells in processing of the particle, and no interference was observed from the presence/absence and type of prebiotic component. MSLs were obtained with relatively uniform spherical surface, and average size between 62.4 ± 2.8 µm to 69.6 ± 5.1 µm, there was no significant difference between formulations. Analyses of X-ray diffraction indicated that there were no polymorphic changes during refrigerated storage of SLMs. As for the thermal analysis it can be said that the presence of probiotics and prebiotics had practically no effect on the melting temperature for all formulations, which was 45.37° C up to 47.58° C, inferring with this the absence of significant interactions between the lipid carrier and microencapsulated ingredients, absence that was reaffirmed by the infrared spectra. Microencapsulation favored the survival against gastric and simulated intestinal fluids, and was possible to maintain viable cells up to 106 CFU per gram up to 120 days of storage for formulation with L. acidophilus and polydextrose in low temperatures and relative humidity (11%), which the stability was influenced by the water activity of the particle, which in turn is affected by the incorporation of prebiotics to the formulation of the SLMs. Given the potential of SLMs developed, they were incorporated into the ice cream. In this matrix microparticles not performed well, either on the survival of L. acidophilus during product storage, such as in protection against exposure to simulated gastrointestinal conditions. Furthermore, the addition of SLMs on strawberry ice cream was evaluated with grades significantly lower (p ≤ 0.05) in the attributes texture, flavor and overall acceptability compared to the control samples and with added of free probiotic sensory analysis of the product developed. The lipid microparticles produced were shown to be suitable as a food ingredient, but the ice cream did not meet the assumptions of protection and extension of appropriate probiotic counts. The MSLs were also incorporated in the fruit pulp, avocado and melon, in this application the SLMs provided protection to the micro-organism increasing the probiotic viability in relation to the free microorganisms

Role of lecithin in oleogel formation : effect of organic phase and study of hybrid systems

Orientadores: Rosiane Lopes da Cunha, António Augusto VicenteTese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de AlimentosResumo: A problemática abordada consiste na proposta de vias alternativas para estruturação convencional de óleos, a qual envolve a formação de redes coloidais cristalinas com altos teores de ácidos graxos trans e/ou saturados. Os oleogéis emergem como alternativa, pois são capazes de promover gelificação de um solvente líquido pela formação de uma rede tridimensional. Para formação de oleogéis à base de fosfolipídios biológicos (lecitinas), em particular a fosfatidilcolina, o hexadecano e triacilgliceróis de cadeia média e longa foram avaliados. Dentre estes somente o hexadecano levou à formação de géis de lecitina. A caracterização da nano e microestrutura, bem como a reológica em condições isotérmicas e não isotérmicas foram investigadas. Os efeitos da concentração de lecitina e inclusão de água ou ácido cítrico (primers) para a modificação do sistema foram avaliados no intuito de melhorar a resposta da força-gel. O entendimento das variáveis envolvidas na formação do gel em sistema modelo foi buscado para que fosse possível a posterior produção de oleogéis com componentes de grau alimentício. Desta maneira, foram propostos sistemas híbridos na presença da lecitina. Foram avaliadas tanto a combinação com ß-sitosterol e 'gama'-orizanol como a interação deste fosfolipídio com diferentes ceras. A mistura lecitina com os fitoesteróis foi investigada por espalhamento de raios-X, microscopia, calorimetria diferencial de varredura, ensaios reológicos e de compressão uniaxial. As unidades estruturais foram se modificando em função da adição de lecitina bem como do tipo de solvente. Comportamentos térmico e mecânico também foram influenciados pela presença da lecitina, que levou à redução da temperatura de fusão, maior tempo necessário para cristalização e aparente redução da dureza do oleogel. Como hipótese propõe-se que a lecitina disputaria sítios de ligação envolvidos na formação dos complexos entre o ß-sitosterol e o 'gama'-orizanol, suprimindo a formação das típicas estruturas fibrilares. No entanto, ainda na busca por um sistema sinérgico envolvendo lecitina, uma varredura com diferentes tipos de cera foi realizada. A cera de frutas, que se destaca por sua singular composição (predominante em ácidos e álcoois graxos), mostrou-se promissora na estruturação de óleos juntamente com a lecitina. Novamente a presença da lecitina afetou o comportamento térmico promovendo um atraso tanto na cristalização da cera como aumentando o tempo requerido para gelificação, além da melhora das propriedades mecânicas (módulo elástico; tixotropia, capacidade de retenção de óleo), em determinadas razões entre os componentes. A lecitina mostrou-se ainda capaz de afetar o hábito cristalino (tamanho e forma) desta cera. Em suma, o trabalho teve inicialmente uma abordagem fundamental para entender a lecitina como agente estruturante, que adiante se corroborou com o estudo de sistemas mais complexos em combinação com outros componentes igualmente vinculados a questão de funcionalidade nutricional e tecnológica. Foram relatados comportamentos dissimilares deste fosfolipídio, ora conferindo maior elasticidade, ora contribuindo com a dureza, como resultado do específico balanço de solubilidade que conduz ao êxito ou não da formação de sistemas gelificados. Desvendar o papel da lecitina, seja como estruturante principal ou secundário, traz a perspectiva em se trabalhar com a engenharia de ingredientes de forma racional e sustentáveAbstract: The proposal of alternative routes for the conventional oil structuring represents an important topic, since conventional routes involve the formation of crystalline colloidal networks that usually are comprised of high levels of saturated and/or trans fatty acids. Oleogels are proposed as alternative because they promote gelation of liquid solvents through 3D network formation. Biological phospholipids (also called lecithins), in particular phosphatidylcholine, were evaluated with different solvents (hexadecane and medium and long chain triacylglycerol) to form oleogels. It was verified that among the studied solvents only hexadecane led to gel formation. The characterization of nano and microstructure and rheological (isothermal and non-isothermal conditions) were investigated. The effect of lecithin concentration and inclusion of water or citric acid (primers) to modify the system were also evaluated in order to optimize the mechanical properties of the gel. The understanding of the variables involved in oleogel formation in a model system was sought so that the production of oleogels with food grade components would be possible from this first stage. Therefore, hybrid systems in the presence of lecithin with other oleogelator(s) were proposed. The combination between lecithin and sterol(ester)s was investigated by small angle X-ray scattering, microscopy, differential scanning calorimetry, rheological and uniaxial compression tests. At nanoscale it was possible to observe that the building blocks were modified according to the addition of lecithin as well as the solvent type. Thermal and mechanical behaviours were also influenced by the presence of lecithin which led to the reduction of the melting temperature, a longer time required for crystallization and the apparent reduction of gel hardness. From these results we hypothesized that lecithin would dispute binding sites involved in the formation of complexes between ß-sitosterol and 'gama'-oryzanol, suppressing the formation of the typical fibrillar structures. However, still in the search for a synergistic system involving lecithin, a scanning with different types of waxes was performed. Among the waxes tested, fruit wax, which stands out for its unique composition (fatty acids and alcohols), showed promising results in oil structuring in combination with lecithin. The presence of lecithin affected the thermal behavior promoting a delay in the crystallization and gelation. An improvement in the mechanical properties (higher elastic modulus, tixotropy and oil binding capacity) at certain ratios between the components was observed when compared with the systems formed only with the wax. Moreover, lecithin affected the crystalline habit (size and shape) of fruit wax. In summary, this study initially had a fundamental approach based on understanding of lecithin as a main oleogelator, and a further investigation of more complex systems focusing in lecithin combined with other components also linked to nutritional and technological functionalities. Dissimilar behaviours of phospholipid either conferring greater plasticity or contributing to the hardness were reported as a result of the specific solubility balance of the system that leads to the success or failure to form gel. Unravelling the role of lecithin as a main or co-oleogelator brings the perspective of working with the engineering of ingredients in a rational and sustainable wayDoutoradoEngenharia de AlimentosDoutora em Engenharia de Alimentos159180/2013-92015/24912-4, 2016/10277-8CNPQFAPES

Role of the oil on glyceryl monostearate based oleogels

The high consumption of saturated and trans fats, used in the formulation of lipid-based foods, is associated with incidence of health problems. Organogels or oleogels are a novel class of structured lipids formed from liquid oil as continuous phase entrapped within network of structuring molecules. The aim of this study was to understand the role of oils with different composition on the formation of glyceryl monostearate (GM) gel network. Glyceryl monostearate-based oleogels were produced with the minimal concentration of 5 wt% in sunflower (SF), high oleic sunflower oil (HOS) and coconut oil (CO). The influence of the oil type on the physicochemical properties of the gel was analyzed. The GM gels showed a solid-like behavior using either high oleic sunflower or sunflower oils but did not form a true gel with coconut oil. Although different oils could affect the crystal formation, all gels exhibited needle-like crystal morphology regardless solvent quality. The GM crystals arranged in a lamellar configuration are responsible for entrapping both SF and HOS oils. Degree of saturation of oils might affect GM oleogel properties. Long chain monounsaturated fatty acids favored the packing of GM crystals in a cohesive gel. Furthermore polymorphism with preferential crystalline beta' form of GM was formed using a medium containing one and two unsaturation. In conclusion, it was observed that the type of oil influenced the formation of the GM gel network. These findings allow the better understanding of GM-based oleogels, providing opportunity to design for food products with improved technological and nutritional properties120610619CONSELHO NACIONAL DE DESENVOLVIMENTO CIENTÍFICO E TECNOLÓGICO - CNPQFUNDAÇÃO DE AMPARO À PESQUISA DO ESTADO DE SÃO PAULO - FAPESP132413/2016-7; 153236/2018-3; 307168/2016-62015/24912-4; 2016/10277-8; 96/08366-5; 2004/08517-3; 2006/03263-9; 2007/58017-5; 2011/06083-

Internal and external factors affecting the crystallization, gelation and applicability of wax-based oleogels in food industry

In recent years, wax-based oleogelation has appeared as a new and effective strategy to structure liquid oil into soft, solid-like systems, which can be exploited as alternatives for trans- and/or saturated lipidic hardstocks in the production of lipid-based food products. Waxes are crystalline gelators, consisting of a mixture of straight chain alkanes, long-chain fatty acids, long-chain fatty alcohols, wax esters, aldehydes, ketones, glycerol esters or di-esters. Wax-based gelation arises from the crystallization of wax particles. Tuning the preparation conditions such as cooling rate, shear rate and setting temperature can alter the crystallization and gelation of natural waxes in liquid oil. A better fundamental understanding on wax-based oleogelation is therefore important to control the quality of food products, in which these oleogels could act as structuring agents. In the food industry, wax-based oleogels can be utilized to partially or fully replace the trans- and/or saturated fats in fat-based food formulations such as shortening, margarine, confectionery products, ice-cream, and whipped-cream. Furthermore, oil migration can be prevented by using wax crystals to capture the free liquid oil within a fat based confectionery filling. The scope of this review is to provide a concise insight into structuring liquid oil using natural waxes, with the emphasis on different internal and external factors affecting the physicochemical properties of wax-based oleogels. The innovative food applications of wax-based oleogels are also discussed in details. Industrial relevance: Wax-based oleogelation has been emerged as a potential alternative to conventional oil structuring. The gelling behavior of natural waxes in liquid oils is governed by the polarity of the solvents, and by the wax crystal morphologies, which are determined by the nature and chain length of the chemical components present in waxes. In addition, the gelling behavior of wax-based oleogels can be tuned by altering the cooling and shear rates, and by changing the time and temperature of cooling. These factors strongly influence the physicochemical properties as well as the storage stability of wax-based oleogels. In addition, the application of wax-based oleogel in food formulations has encountered some technical challenges due to the incompatibility between oleogels and saturated fats, and due to the insufficient amount of solid content provided by waxes. With regard to the sensorial aspect, the waxy mouthfeel might be an obstacle restricting the acceptance of wax-based products in food markets. This review therefore provides a concise overview relating to the internal (chemical composition of natural waxes, type and polarity of solvents) and external factors (cooling rate, shear rate, storage time, and co-structuring) affecting the crystallization and gelation of wax-based oleogels, as well as their potential application in producing low-saturated fat products in food industry

Technological Challenges for Spray Chilling Encapsulation of Functional Food Ingredients

Hlađenje se raspršivanjem (ili zamrzavanje raspršivanjem) već godinama detaljno proučava i upotrebljava u farmaceutici. U prehrambenoj industriji raste interes za primjenom ove tehnike, jer se pomoću nje mogu razviti funkcionalni prehrambeni proizvodi. Pri hlađenju se raspršivanjem sastojak dodaje u otopljeni lipidni nosač, a dobivena se smjesa raspršuje kroz mlaznicu atomizatora. Kada raspršeni materijal dođe u kontakt s okolinom, koja je ohlađena na temperaturu nižu od tališta nosača, sastojak se zgušnjava zbog izmjene topline između otopljenog materijala i hladnoga zraka, pri čemu nastaju čvrste lipidne mikročestice. Tehnologija se temelji na uporabi lipidnih nosača, kao što su voskovi i masti (npr. palmino ulje, pčelinji vosak, kakao maslac i ulje palminih koštica). Enkapsuliranjem se može promijeniti funkcionalnost, smanjiti higroskopnost, prikriti miris i okus, promijeniti topljivost sastojka te osigurati njegova zaštita, pri čemu se omogućuje kontrolirano otpuštanje aktivne komponente. Ova se jeftina tehnologija može relativno jednostavno koristiti i u industrijskim omjerima, a ne zahtijeva primjenu organskih otapala i povišene temperature. Enkapsulacija hlađenjem pomoću raspršivanja može ubrzati razvoj i proizvodnju funkcionalne i obogaćene hrane, jer može riješiti neke tehnološke probleme vezane uz uporabu sastojaka velike reaktivnosti i male stabilnosti.Spray chilling technology (also known as spray cooling and spray congealing technology) has been widely studied and used in the pharmaceutical field. In the food industry, this technique is gaining interest and can become useful because functional food formulations can be developed. Spray chilling is a fat-based system, which involves the addition of the component of interest to a molten lipid carrier, and the resulting mixture is fed through an atomiser nozzle. When the nebulised material is put into contact with the environment, which is cooled below the melting point of the matrix material, the vehicle solidifies (due to heat exchange between the molten material and cold air), and solid lipid microparticles are formed at the same time. This technology is fat based, and lipid carriers, such as wax and oil (e.g. palm oil, beeswax, cocoa butter, and kernel oil) can be used. This encapsulation technique can potentially change the functionality, reduce the hygroscopicity, mask taste or odour, change solubility, and provide physical protection in addition to allowing the controlled release of these ingredients. This low-cost technology is relatively simple to apply and scale up, and it does not require the use of organic solvents and the application of high temperatures in the process. Therefore, spray chilling encapsulation may facilitate the development and production of functional and enriched foods as it may solve some technological problems associated with the use of certain ingredients, such as those that have high reactivity and low stability

Chia (Salvia hispanica L.) mucilage as a new fat substitute in emulsified meat products: Technological, physicochemical, and rheological characterization

The objective of the study was to evaluate the rheological properties of chia mucilage (CM) gels as functional ingredient in emulsified meat model systems. Three different concentrations of chia mucilage gels (CMGs) (15%, 20%, and 25%), were applied in two levels (2.5% and 5.0%), aiming to substitute 50% of pork back fat in the meat model systems. Two control treatments (FC1 and FC2 containing 20 and 10% fat, respectively) were also tested. The rheological behavior of the mucilage was viscoelastic with a dominant storage modulus (G’ > G”) forming a structure type gel. The values of tan δ ranged between 0.37 and 0.40, which could indicate a weak elastic gel-like behavior in the frequency range studied. The mechanical properties of CMGs were preserved after thermal treatment. The meat emulsion stability was improved with the addition of CMG. All formulations with 5% CM were characterized by significantly increased hardness, and decreased elasticity and cohesiveness values (P < 0.05) compared to those with FC1. Chia mucilage thus shows potential as a substitute saturated fat (SFA) in emulsified meat products with improved technological characteristics and additional healthier claims.This work was supported by the National Council for Scientific and Technological Development (CNPq) [grant number 140854/2016-9] and the Foundation for Research Support of the State of São Paulo (FAPESP) [grant number 2016/19967-7].Peer reviewe

Whey protein as a key component in food systems: physicochemical properties, production technologies and applications

Whey protein is a potential and versatile ingredient in the development of novel and natural component in food products. It can work as a texture modifier, thickening agent, carrier/vehicle, gelling agent, surface-active component, and foaming agent among other associated functionalities and bioactivities. Nanocomposites containing whey proteins, for example, have been used as effective encapsulation systems of active food and drug components, enhancing their solubility, transport, dispersibility, bioavailability and bioaccessibility. This review provides an overview of the functional and biological properties of whey protein as a key component in food systems, focusing on their physicochemical/structural characteristics, production technologies and applications.14172

Understanding the role of chia (Salvia Hispanica L.) mucilage on olive oil-based emulsion gels as a new fat substitute in emulsified meat products

This study aimed to develop a chia mucilage (MC)-based emulsion gel (EG) with olive oil to replace pork back fat in emulsified meat products. Six variables (alginate—ALG; collagen—COL; whey—WHEY; carboxymethylcellulose—CMC; transglutaminase—MTG; carrageenan—CAR) with MC were evaluated using a Plackett–Burman (PB) design. Then, a complete factorial design was applied to evaluate the interactions and properties of the selected variables (ALG, COL, and WHEY) for the manufacture of EGs. The responses evaluated in the EGs were pH, color, emulsion stability, rheological, and texture parameters. In PB, the variables CMC, COL, ALG, and WHEY did not lead to any significant effects on the pH values of EGs, which ranged from 5.6 to 5.8. WHEY had a significant effect on the increase in luminosity of the EGs. ALG and WHEY decreased the liquid release of the samples showing greater stability of EGs and meat model systems. All samples of EGs, apart from run 5 (CMC, MTG, CAR, and ALG), showed a typical gel-like behavior (Gʹ > Gʺ) and a frequency-independent behavior. Even the formulation with only mucilage (run 12) showed a dominant Gʹ forming a gel-like structure. The complete factorial design showed stable and strong interactions between WHEY, MC, and olive oil, since a small or no liquid release, were observed in all experiments with WHEY. This study contributed to understanding the interactions among MC, biopolymers, and proteins, disclosing the potentiality of chia mucilage-based emulsion gels for the replacement of animal fat in emulsified meat products.The authors thank National Council for Scientific and Technological Development (CNPq) and Foundation for Research Support of the State of São Paulo (FAPESP) (process numbers 140854/2016-9 and 2016/19967-7, respectively) for the financial support to this work and scholarships. This study was financed in part by the Coordenação de Aperfeiçoamento de Pessoal de Nível Superior-Brazil (CAPES)-Finance Code 001.Peer reviewe