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Lactobacillus delbrueckii subsp. bulgaricus and Lactiplantibacillus plantarum are two lactic acid bacteria (LAB) widely used in the food industry. The objective of this work was to assess the resistance of these bacteria to freeze- and spray-drying and study the mechanisms involved in their loss of activity. The culturability and acidifying activity were measured to determine the specific acidifying activity, while membrane integrity was studied by flow cytometry. The glass transitions temperature and the water activity of the dried bacterial suspensions were also determined. Fourier transform infrared (FTIR) micro-spectroscopy was used to study the biochemical composition of cells in an aqueous environment. All experiments were performed after freezing, drying and storage at 4, 23 and 37 °C. The results showed that Lb. bulgaricus CFL1 was sensitive to osmotic, mechanical, and thermal stresses, while Lpb. plantarum WCFS1 tolerated better the first two types of stress but was more sensitive to thermal stress. Moreover, FTIR results suggested that the sensitivity of Lb. bulgaricus CFL1 to freeze-drying could be attributed to membrane and cell wall degradation, whereas changes in nucleic acids and proteins would be responsible of heat inactivation of both strains associated with spray-drying. According to the activation energy values (47-85 kJ/mol), the functionality loss during storage is a chemically limited reaction. Still, the physical properties of the glassy matrix played a fundamental role in the rates of loss of activity and showed that a glass transition temperature 40 °C above the storage temperature is needed to reach good preservation during storage. KEY POINTS: • Specific FTIR bands are proposed as markers of osmotic, mechanic and thermal stress • Lb. bulgaricus CFL1 was sensitive to all three stresses, Lpb. plantarum WCFS1 to thermal stress only • Activation energy revealed chemically limited reactions ruled the activity loss in storage.

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A new optical method for assigning glass viscosity values in the softening temperature range is presented. In this method, an irregular particle, a few millimeters in size, laying on an alumina plate, is heated up to temperature T, and then remains at this temperature. T should be within the softening temperature range of the glass. There are no external applied shear stresses, the only acting shear forces are those coming from the particle's own surface energy. At the fixed temperature T, the surface free energy of the sample decreases by viscous flow while its shape evolves from a polyhedron or irregular shape towards a spherical or rounded shape. This shape evolution is recorded using a photographic camera. From each image, the sample's roundness is determined, obtaining a characteristic time τ from the roundness against time. Simultaneously, using the available software, a value for the viscosity η was calculated, at temperature T, allowing for building sets of T, τ, η, namely three data values. Accordingly, if T, τ are considered as independent variables, a master function η = η (T, τ) can be built. Now, if we measure T, τ data on a glass of an unknown viscosity, the master function makes it possible to assign a η value. When incipient crystallization or liquid-liquid phase separations are present, effective viscosity values are obtained. This method requires a high temperature microscope, as well as tridimmensional samples with a few cubic millimeters of volume. Each isothermal τ determination can take from minutes to several hours. We tested the method with two glasses of known viscosity values: borosilicate glass (VG98) and alumimoborosilicate glass (SG7), both of which are used for radioactive waste immobilization and have assigned log(η) values between 6 and 7.3 with η in Pa s. The discrepancy between the log(η) values assigned here and those values fitted with a VFT function on the values measured for the SG7 and VG98 glasses were within ±14%.

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In this study, the effects of different concentrations of pea protein concentrate (PPC) in the physical properties, porosity features, and oxidative stability of maltodextrin-based spray-dried microparticles containing orange essential oil (OEO, rich in limonene) were evaluated. The use of PPC resulted in spray-dried microparticles with encapsulation efficiencies of about 99 wt%, without visible pores, and relatively high glass transition temperature (66,4 °C) at Aw âˆ¼ 0.3. The nitrogen adsorption and positron annihilation lifetime spectroscopy measurements showed that the increase of PPC concentration from 2.4 to 4.8 wt% (g of PPC/100 g of emulsion) did not affect the porosity features of the microparticles. These results were confirmed by the profiles of OEO retention and limonene oxide production, which were similar for both samples throughout four weeks of storage. Based on these results, we verified that the lower amount of PPC we tested can effectively protect the OEO during storage, showing that a relatively cheaper orange flavor powder can be produced using less protein.

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Inulin-type fructans with different degrees of polymerization (DPs) were used as wall materials for the blue colorant produced from the crosslinking between genipin and milk proteins. The impact of using fructooligosaccharides (FOS) with DP = 5 and inulins with DP ≥ 10 (GR-In) and DP ≥ 23 (HP-In) on the physical (microstructure, size, water activity, wettability, solubility, water adsorption, glass transition temperature, and color), chemical (free genipin retention and moisture), and technological (colorant power, pH stability, and thermal stability) properties of the powdered blue colorant was examined. Inulins were more efficient carriers as seen from the physical characteristics of the microparticles. FOS and GR-In promoted higher retention of free genipin than HP-In. Additionally, their lower DP influenced the rehydration proprieties as well as the color intensity and colorant power. The DP did not affect the physical stability of the colorant at different pH conditions or at high temperature. Our findings demonstrated that the DP of the fructan exhibited a strong impact on the blue intensity of the samples and also their rehydration capacity.

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Materials that have high dielectric constants, high energy densities and minimum dielectric losses are highly desirable for use in capacitor devices. In this sense, polymers and polymer blends have several advantages over inorganic and composite materials, such as their flexibilities, high breakdown strengths, and low dielectric losses. Moreover, the dielectric performance of a polymer depends strongly on its electronic, atomic, dipolar, ionic, and interfacial polarizations. For these reasons, chemical modification and the introduction of specific functional groups (e.g., F, CN and R-S(=O)2-R´) would improve the dielectric properties, e.g., by varying the dipolar polarization. These functional groups have been demonstrated to have large dipole moments. In this way, a high orientational polarization in the polymer can be achieved. However, the decrease in the polarization due to dielectric dissipation and the frequency dependency of the polarization are challenging tasks to date. Polymers with high glass transition temperatures (Tg) that contain permanent dipoles can help to reduce dielectric losses due to conduction phenomena related to ionic mechanisms. Additionally, sub-Tg transitions (e.g., γ and ß relaxations) attributed to the free rotational motions of the dipolar entities would increase the polarization of the material, resulting in polymers with high dielectric constants and, hopefully, dielectric losses that are as low as possible. Thus, polymer materials with high glass transition temperatures and considerable contributions from the dipolar polarization mechanisms of sub-Tg transitions are known as "dipolar glass polymers". Considering this, the main aspects of this combined strategy and the future prospects of these types of material were discussed.

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This research work aimed to obtain blackberry pulp powder by spray drying and, by an experimental design, evaluated the effect of inlet air temperature (100-150 °C) and blackberry pulp solids:arrowroot starch/gum arabic solids ratio of 1:0.5-1:2 on the physicochemical properties of the powders. Arrowroot starch and gum arabic present glass transition temperature (Tg) values above 100 °C; hence it was possible to employ them as carriers in blackberry pulp spray drying in order to increase Tg of the system. Powder yield and solubility increased with increasing blackberry pulp solids:arrowroot starch/gum arabic solids ratio of 1:0.5-1:2, whereas hygroscopicity decreased. Yield, solubility and hygroscopicity of the powders increased and water activity decreased, with increasing inlet air temperature. The powders presented low moisture content and water activity. Temperature of 143 °C and blackberry pulp solids:arrowroot starch/gum arabic solids ratio of 1:1.78 were the optimal conditions to obtain high yield and blackberry powders that are soluble in water and less hygroscopic.

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Spray dryer was used to produce particles from a milk-blackberry pulp mixture (25%:75% (w/w)). Maltodextrin 10DE and 20DE and gum Arabic were used as adjuvants in order to improve powder quality. The particles were analyzed with emphasis on physical and physicochemical characteristics: moisture content, bulk density, particle size, morphology, water activity, anthocyanins retention, anthocyanins content, hygroscopicity, solubility, water sorption, and glass transition temperature. The best results were obtained for the paste composition of 25% concentrated milk-70% blackberry pulp-5% gum Arabic, yielding high anthocyanins retention (>87.5%), low powder moisture content of 0.0265 g H2 O/g dry matter and a higher powder solubility (>71.8%) when compared with other formulations. The increase of water content led to a decrease of powder's glass transition temperature. Powder stability was evaluated and the critical values of relative humidity and moisture content were estimated based on state diagrams of glass transition combined with sorption isotherm data. PRACTICAL APPLICATION: The growing interest in blackberries is due to the presence of anthocyanins which have shown possible application as a natural dye for food and pharmaceutical products. Drying a mixture of blackberry pulp and milk may produce particles with a broad range of intrinsic nutrients. Milk components could act as a wall material and emulsifying agent, protecting the flavonoids from blackberry. Therefore, a milk-blackberry powder becomes an alternative, which may reduce postharvesting waste and increase the shelf life of the product without significantly altering its nutritional characteristics.

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In this work is presented the complete thermal analysis of polyols by direct methods such as simultaneous thermogravimetric and differential thermal analyzer (TGA-DTA), differential scanning calorimetry (DSC), modulated DSC (MDSC), and supercooling MDSC. The different thermal events in the temperature range of 113⁻553 K were identified for glycerol (GL), ethylene glycol (EG), and propylene glycol (PG). Boiling temperature (TB) decreased as GL > EG > PG, but increased with the heating rate. GL showed a complex thermal event at 191⁻199 K, identified as the glass transition temperature (Tg) and devitrification temperature (Tdv), and a liquid⁻liquid transition (TL-L) at 215⁻221 K was identified as the supercooling temperature. EG showed several thermal events such as Tg and Tdv at 154 K, crystallization temperature (Tc) at 175 K, and melting temperature (Tm) at 255 K. PG also showed a complex thermal event (Tg and Tdv) at 167 K, a second devitrification at 193 K, and TL-L at 245 K. For PG, crystallization was not observed, indicating that, during the cooling, the liquid remained as an amorphous solid.

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In this work maltodextrins were added to commercial galacto-oligosaccharides (GOS) in a 1:1 ratio and their thermophysical characteristics were analyzed. GOS:MD solutions were then used as matrices during spray-drying of Lactobacillus plantarum CIDCA 83114. The obtained powders were equilibrated at different relative humidities (RH) and stored at 5 and 20°C for 12 weeks, or at 30°C for 6 weeks. The Tgs of GOS:MD matrices were about 20-30°C higher than those of GOS at RH within 11 and 52%. A linear relation between the spin-spin relaxation time (T2) and T-Tg parameter was observed for GOS:MD matrices equilibrated at 11, 22, 33, and 44% RH at 5, 20, and 30°C. Spray-drying of L. plantarum CIDCA 83114 in GOS:MD matrices allowed the recovery of 93% microorganisms. In contrast, only 64% microorganisms were recovered when no GOS were included in the dehydration medium. Survival of L. plantarum CIDCA 83114 during storage showed the best performance for bacteria stored at 5°C. In a further step, the slopes of the linear regressions provided information about the rate of microbial inactivation for each storage condition (k values). This information can be useful to calculate the shelf-life of spray-dried starters stored at different temperatures and RH. Using GOS:MD matrices as a dehydration medium enhanced the recovery of L. plantarum CIDCA 83114 after spray-drying. This strategy allowed for the first time the spray-drying stabilization of a potentially probiotic strain in the presence of GOS.

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This work studies how sucrose (S) addition modifies the thermal properties of cassava starch (CS). Neat CS and CS-S blends with 4, 6 and 8% sugar contents (CS-S-4%, CS-S-6% and CS-S-8%) were prepared and analyzed by differential scanning calorimetry (DSC) and dynamic mechanical thermal analysis (DMTA), in a wide range of moisture levels (2-20%). In equilibrated samples with moisture contents lower than 10%, twoendothermic steps were observed during first DSC heating scans and two corresponding relaxation maxima in tan δ were detected by DMTA. The first transition, detected at around 45-55°C by both DSC and DMTA, is frequently found in starchy foods, while the second observed at higher temperatures is associated to the glass transition temperature of the blends. At higher moisture contents, only one thermal transition was observed. Samples analyzed immediately after cooling from the melt (i.e., after erasing their thermal history), exhibited a single glass transition temperature, regardless of their moisture content. Addition of sugar promotes water plasticization of CS only at high moisture contents. In the low moisture content range, anti-plasticization was observed for both neat and sugar-added CS samples. Addition of sugar decreases the moisture content needed to achieve the maximum value of the glass transition temperature before plasticization starts. The results of this work may be valuable for the study of texture establishment in low moisture content extruded food products.

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Physicochemical properties and structural characteristics of whole rice flours with different treatments (soaking, germination and extrusion cooking) were studied. Water solubility, water absorption, crystallinity, adsorption isotherms (BET and GAB models), and glass transition temperature of the samples were determined. Water solubility and water absorption were enhanced by extrusion cooking process (3.17-4.98 vs. 24.1-53.76 g/100 g and 2.77-3.05 vs. 4.46-7.04 ml/g, respectively), but crystallinity was decreased (30-33 vs. 4-16%). Adsorption isotherms showed that extruded samples exhibited higher equilibrium moisture content as compared with their corresponding non-extruded samples (5.0-19.2 vs. 4.0-16.1 g water/g solids). There were no changes in glass transition temperature values in the studied moisture range (3.8-16 g/100 g). These results allow the correct use of whole rice flours with different treatments in foods and also contributed to the knowledge of stabilization of the products.

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BACKGROUND: The search for natural, novel, high-quality, stable food ingredients is an ongoing practice in the food industry. Pulp of borojo (Borojoa patinoi Cuatrecasas), which is a fruit of the Colombian Pacific region, can be separated into three phases: liquid (LP), medium (MP) and solid (SP) phases. The objective of this work was to evaluate the effect of the three-phase composition and gum arabic on their glass transitions temperatures (T(g)). The best mixture, LP-MP, MP-SP and LP-SP and gum arabic (GA) was identified by response surface methodology. RESULTS: When adding GA to SP borojo phase in a 1:1 proportion, the resulting T(g) of the mixture was 132.27 °C whereas Tg for GA and SP-phase were 154.89 °C and 79.86 °C respectively, which supported this combination as attractive from a processing perspective and supports an industrial advantage of using borojo as food ingredient. Phases were characterized by high-performance liquid chromatography, Fourier transform infrared spectroscopy, confocal laser scanning microscopy and mass spectrometry. Low molecular weight compounds such as fructose for MP lowered T(g) whereas the presence of lignin increased T(g) of the mixtures as with the SP. CONCLUSIONS: The addition of GA significantly increased T(g) of borojo phases so leading to propose them as novel food processing materials.

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Maltodextrin (MX) is an ingredient in high demand in the food industry, mainly for its useful physical properties which depend on the dextrose equivalent (DE). The DE has however been shown to be an inaccurate parameter for predicting the performance of the MXs in technological applications, hence commercial MXs were characterized by mass spectrometry (MS) to determine their molecular weight distribution (MWD) and degree of polymerization (DP). Samples were subjected to different water activities (aw). Water adsorption was similar at low aw, but radically increased with the DP at higher aw. The decomposition temperature (Td) showed some variations attributed to the thermal hydrolysis induced by the large amount of adsorbed water and the supplied heat. The glass transition temperature (Tg) linearly decreased with both, aw and DP. The microstructural analysis by X-ray diffraction showed that MXs did not crystallize with the adsorption of water, preserving their amorphous structure. The optical micrographs showed radical changes in the overall appearance of the MXs, indicating a transition from a glassy to a rubbery state. Based on these characterizations, different technological applications for the MXs were suggested.

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ß-Cyclodextrin (ß-CD)-grafted dextrans with spacer arms of different length were employed to evaluate the impact of supramolecular interactions on invertase activity. The modified dextrans were used as single additives or combined with trehalose in freeze-dried formulations containing invertase. Enzyme activity conservation was analyzed after freeze-drying and thermal treatment. The change of glass transition temperature (Tg ) was also evaluated and related to effective interactions. Outstanding differences on enzyme stability were mainly related to the effect of the spacer arm length on polymer-enzyme interactions, since both the degree of substitution and the molecular weight were similar for the two polymers. This change of effective interactions was also manifested in the pronounced reduction of Tg values, and were related to the chemical modification of the backbone during oxidation, and to the attachment of the ß-CD units with spacer arms of different length on dextran.

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Freeze-dried chia mucilage adsorption isotherms were determined at 25, 35 and 40°C and fitted with the Guggenheim-Anderson-de Boer model. The integral thermodynamic properties (enthalpy and entropy) were estimated with the Clausius-Clapeyron equation. Pore radius of the mucilage, calculated with the Kelvin equation, varied from 0.87 to 6.44 nm in the temperature range studied. The point of maximum stability (minimum integral entropy) ranged between 7.56 and 7.63kg H2O per 100 kg of dry solids (d.s.) (water activity of 0.34-0.53). Enthalpy-entropy compensation for the mucilage showed two isokinetic temperatures: (i) one occurring at low moisture contents (0-7.56 kg H2O per 100 kg d.s.), controlled by changes in water entropy; and (ii) another happening in the moisture interval of 7.56-24 kg H2O per 100 kg d.s. and was enthalpy driven. The glass transition temperature Tg of the mucilage fluctuated between 42.93 and 57.93°C.

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In this work two systems based on a carbohydrate polymer were studied: inulin as model system and inulin-orange juice as complex system. Both system were stored at different water activity conditions and subsequently characterized. Water adsorption isotherms type II were fitted by the GAB model and the water monolayer content was determined for each system. From thermal analyzes it was found that at low water activities (aw) systems were fully amorphous. As aw increased, crystallinity was developed. This behavior was corroborated by X-ray diffraction. In the inulin-orange juice system, crystallization appears at lower water activity caused by the intensification of the chemical interaction of the low molecular weight species contained in orange juice. Glass transition temperature (Tg), determined by modulated differential scanning calorimeter, decreased with aw. As water is adsorbed, the physical appearance of samples changed which could be observed by optical microscopy and effectively related with the microstructure found by scanning electron microscopy.

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Glass transition temperatures and physical aging of amorphous cassava starch and their blends with corn oil were assessed by differential scanning calorimetry (DSC). Two enthalpic relaxation endotherms, well separated in temperature values, were exhibited by neat amorphous cassava starch with 10.6% moisture content, evidencing two amorphous regions within the starch with different degrees of mobility. The phase segregation of these two amorphous regions was favored by added corn oil at low moisture contents during storage. The presence of amylose-lipid complexes in this matrix, may also affect the molecular dynamics of these two amorphous regions at low moisture contents. Increasing moisture content, leads to a homogeneous amorphous phase, with an aging process characterized by a single enthalpic relaxation peak. In all cases, after deleting the thermal history of the samples only one glass transition temperature was detected (during DSC second heating runs) indicating that a single homogeneous amorphous phase was attained after erasing the effects of physical aging. Trends of the enthalpic relaxation parameters were also different at the two moisture contents considered in this work.

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Valeriana officinalis L. (Valerianaceae) is one of the most widely used plants for the treatment of anxiety and insomnia. Usually dry plant extracts, including V. officinalis, are hygroscopic materials with poor physico-mechanical properties that can be directly compressed.A V. officinalis dry extract with moderate hygroscocity is suitable for direct compression, and was obtained by using a simple and economical technique. The V. officinalis fluid extract was oven-dried with colloidal silicon dioxide as a drying adjuvant. The addition of colloidal silicon dioxide resulted in a dry plant extract with good physico-mechanical properties for direct compression and lower hygroscopicity than the dry extract without the carrier. The dry plant extract glass transition temperature was considerably above room temperature (about 72 °C). The colloidal silicon dioxide also produced an antiplasticizing effect, improving the powder's physical stability.The pharmaceutical performance of the prepared V. officinalis dry extract was studied through the design of tablets. The manufactured tablets showed good compactability, friability, hardness, and disintegration time. Those containing a disintegrant (Avicel PH 101) exhibited the best pharmaceutical performance, having the lowest disintegration time of around 40 seconds.

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The Eucalyptus grandis logs temperatures were determined and correlated with the board's cracks during steaming. Thermocouples were inserted in the logs center, registering their temperatures during steaming at 90"C. The logs were sawed and the board's cracks measured. It was concluded that: (1) the logistic S-shaped curve explains the logs temperature variation; (2) the logs with diameter of 20 to <25, 25 to <30 and 30 to <35 cm presented, respectively, 84.2"C, 73.1"C and 45.8"C in the steaming; and (3) the cracks lengths significantly decreased in logs that reached the glass transition temperature.

As temperaturas em toras de Eucalyptus grandis, durante a vaporização, foram determinadas e correlacionadas com as rachaduras das tábuas. Nos centros das toras foram inseridos termopares e registradas suas temperaturas durante a vaporização à 90"C. As toras foram desdobradas e as rachaduras das tábuas mensuradas. Concluiu-se que: (1) o modelo estatístico sigmoidal logístico explica a variação da temperatura nas toras; (2) as toras com 20 a <25, 25 a <30 e 30 a <35 cm de diâmetro apresentaram, respectivamente, 84,2"C, 73,1"C e 45,8"C ao final da vaporização; e (3) as rachaduras foramsignificativamente menores nas toras que atingiram a temperatura de transição vítrea.

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INTRODUCCIÓN: para la obtención en forma de polvo de los extractos y jugos de origen vegetal se emplea el secado por aspersión, porque es un método que preserva los componentes naturales presentes en estos productos. La presencia de compuestos como los azúcares impiden que estos puedan ser secados por aspersión sin que se adhieran a las superficies internas del equipo, lo que trae como consecuencia el bajo rendimiento en la recuperación del producto. El uso de aditivos inertes como el almidón soluble, celulosa o maltodextrina, favorece la recuperación del producto, elevando la temperatura de transición vítrea. OBJETIVOS: aplicar herramientas para el diseño del proceso de secado por aspersión de extractos de plantas. MÉTODOS: se determinaron las temperaturas de transición vítrea de diferentes extractos por calorimetría de barrido diferencial. Se calcularon las temperaturas de apelmazamiento y los índices individuales de secado. RESULTADOS: se determinó, que el uso de aditivos en el proceso de secado por aspersión de extractos de plantas permite obtener extractos en polvo en aquellos casos que no es posible secarlos solos. La metodología empleada, puede ser aplicada a distintos extractos. CONCLUSIONES: se demostró la factibilidad de la metodología propuesta como herramienta para definir la concentración de coadyuvante del secado y las temperaturas de secado

INTRODUCTION: to obtain extracts and juices of vegetal origin as powders, it is necessary to use the spray drying because this method preserves the natural compounds present in these products. Compounds like sugars prevent them from being spray dried without sticking to the inner surfaces of the dryer, all of which results in poor product recovery. The use of inert additives as soluble starch, cellulose or maltodextrin, favors the product recovery by increasing the glass transition temperature. OBJECTIVES: to use design tools for plant extract spray drying process. METHODS: the glass transition temperature was estimated for different extracts by differential scanning calorimetry. Sticking temperature as well as individual drying indexes were calculated. RESULTS: it was demonstrated that the use of additives in plant extract spray drying processes allows obtaining powdered extracts when it is not possible to dry the extract alone. This methodology can be applied to various extracts. CONCLUSIONS: the feasibility of the submitted methodology as a tool for defining adjuvant concentration and drying temperatures was shown

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