Formulation factors affecting foam properties during vacuum foam-drying.

This paper explores how vacuum foam-drying of a protein is influenced by formulation parameters by investigating the foam structure, physical properties of the foam, and the stability of the protein. Recombinant human bile salt-stimulated lipase was used as a model of a protein drug. The stability of the lipase was evaluated through activity measurements. Two disaccharides (sucrose and trehalose), strongly tending to an amorphous form, were used as matrix formers, and the physical properties were assessed through residual water content, glass transition temperature, and crystalline state. Moreover, some formulations included surfactants with different sizes and structures of the head group. The alkyl chain length was kept constant to only investigate the impact of the surfactant head group, in the presence of the lipase, on the foamability and surface coverage of the lipase. The study demonstrated that the lipase allowed for a dry, solid foam with a foam overrun of up to 2600 %. The wall thickness of the dry, solid foam was estimated to be 20-50 µm. Clear differences between sucrose and trehalose as matrix former were identified. The lipase showed no tendency to lose activity because of the drying and rehydration, despite a proportion of the lipase covering the surfaces of the dry material.

Comparison of the Chemical Composition of Six Canihua (Chenopodium pallidicaule) Cultivars Associated with Growth Habits and after Dehulling.

The canihua (Chenopodium pallidicaule) is a native Andean crop that stands out for its high content of protein, fiber, and minerals and that has a good fatty acid profile. We studied six canihuas cultivars, which were compared according to their proximate, mineral, and fatty acid composition. Based on the form of stems, termed growth habit, they belonged to two groups: decumbent (Lasta Rosada, Illimani, Kullaca, and Cañawiri) and ascending (Saigua L24 and Saigua L25). Dehulling is an important process applied to this grain. However, there is no information about how it affects the chemical composition of the canihua. Dehulling resulted in two levels, whole and dehulled canihua. The highest protein and ash contents were in whole Saigua L25 (19.6 and 5.12 g/100 g, respectively), and the highest fat content was found in dehulled Saigua L25, while the whole grains of Saigua L24 presented the highest fiber content (12.5 g/100 g). Dehulling mainly affected the macro-minerals content, while micro-minerals were only slightly linked to the dehulling. The growth habit influenced the C18:1 and C18:3 contents. In conclusion, the canihua had a nutritional composition influenced by each variety, strongly influenced by dehulling, and to a lesser extent by growth habit.

Oil-Based Delivery Control Release System Targeted to the Later Part of the Gastrointestinal Tract-A Mechanistic Study.

Oil-based drug delivery systems have been studied in different aspects. The present study proposes a new application for an oil-based delivery system, focusing on controlled release until the drug reaches the later part of the small intestine. Bulk surfactants and interfacial surfactants were added into the oil formulation to provide a better mechanistic understating of the lipolysis. Validation of the modified in vitro method shows the overall conversion from medium-chain triglyceride oil (MCT oil) to free fatty acids (FFA) of 100 ± 4% in five replicates. This fully converted level and high reproducibility are fundamental for the following investigations where any retarding effect can be distinguished from the experimental errors. The results show that viscosity and thermodynamic activity have limited retardation. Furthermore, the former may change the kinetics of lipolysis, while the latter changes the equilibrium level. The gel-forming retarder (ethylcellulose) displayed a strong effect. Whereas the lipolysis was significantly retarded (>50%) when the retarders altered the interfacial composition (poloxamer 407), degradable interfacial surfactants did not have the same effect. However, surface-active, lipolysis-resistant retarders with a high CMC did not show a retarding effect.

Characterization on the impact of different clarifiers on the white wine colloids using Asymmetrical Flow Field-Flow Fractionation.

Clarifiers are substances used during the winemaking process to enhance clarity and stability in the wines. The different clarifiers may alter removal capacities differently. In this study, the removal efficiency of seven common fining agents, divided into three groups (mineral clarifiers, synthetic polymeric clarifiers, and vegetable protein clarifiers), was analyzed with Asymmetrical Flow Field-Flow fractionation (AF4). Besides, the relationship between the removal capacity and different molecular and macromolecular properties has been evaluated. The results showed extensive removal of colloidal and macromolecular matter by the bentonites with potential impact on characteristic properties of the wine. The vegetable clarifiers showed a more profiled reduction, potentially preserving characteristics of the wine. The synthetic polymers showed a more limited removal efficiency but with a high affinity to remove colloidal phenols. The use of AF4-UV-MALS-dRI allowed the characterization of the wines after different clarification treatments, showing to be an analytical technique with a potential impact on the wine industry.

Flow cytometric analysis reveals culture condition dependent variations in phenotypic heterogeneity of Limosilactobacillus reuteri.

Optimisation of cultivation conditions in the industrial production of probiotics is crucial to reach a high-quality product with retained probiotic functionality. Flow cytometry-based descriptors of bacterial morphology may be used as markers to estimate physiological fitness during cultivation, and can be applied for online monitoring to avoid suboptimal growth. In the current study, the effects of temperature, initial pH and oxygen levels on cell growth and cell size distributions of Limosilactobacillus reuteri DSM 17938 were measured using multivariate flow cytometry. A pleomorphic behaviour was evident from the measurements of light scatter and pulse width distributions. A pattern of high growth yielding smaller cells and less heterogeneous populations could be observed. Analysis of pulse width distributions revealed significant morphological heterogeneities within the bacterial cell population under non-optimal growth conditions, and pointed towards low temperature, high initial pH, and high oxygen levels all being triggers for changes in morphology towards cell chain formation. However, cell size did not correlate to survivability after freeze-thaw or freeze-drying stress, indicating that it is not a key determinant for physical stress tolerance. The fact that L. reuteri morphology varies depending on cultivation conditions suggests that it can be used as marker for estimating physiological fitness and responses to its environment.

Fractionation of Nanoparticle Matter in Red Wines Using Asymmetrical Flow Field-Flow Fractionation.

The particle matter of wine is mainly composed of wine colloids and macromolecules. The present work develops a methodology using asymmetrical flow field-flow fractionation coupled with multi-angle light scattering, differential refractive index detector, and ultraviolet detector (AsFlFFF-MALS-dRI-UV) for the fractionation and determination of the molar mass, the hydrodynamic radius, and the apparent densities of the aggregates and macromolecules present in wine samples. The results from a set of six Argentinian high-altitude wines showed two main populations: the first population composed of wine colloids with higher UV-specific absorptivity and the second population composed of polysaccharides, such as arabinogalactans. The conformation results showed that population 1 consists of small and dense particles, while population 2 showed high molar masses and lower densities. The results demonstrated the use of AsFlFFF as a new, effective method for the fractionation and characterization of wine colloids and wine macromolecules in red wines with further potential applications.

Phytate, iron, zinc, and calcium content of common Bolivian foods and their estimated mineral bioavailability.

There is a scarcity of information on mineral and phytate content in plant-based foods in Bolivia. This study aimed to analyze iron, zinc, calcium, and phytate content and estimate the mineral bioavailability of foods consumed in Chapare, Bolivia. Minerals and phytate were analyzed, and bioavailability was estimated in 17 food samples. Leafy vegetables and green legumes had the highest mineral content, followed by pseudocereals. Estimated mineral bioavailability was low for cereals, dry legumes, pseudocereals, and flaxseeds foods mainly due to phytate content. But estimated zinc bioavailability for black cornmeal, yellow corn, and dry peas was moderate. Strong correlations (p < 0.01) were found between the three minerals, while phytate correlated negatively to iron, zinc, and calcium. To get an overview of the estimated mineral bioavailability of plant-based diets, we have included foods, from the same area, analyzed in a previous study where the evaluated diet covers 80% of RNI for iron and zinc, but <40% of calcium. In conclusion, leafy vegetables and green legumes had the highest contents of minerals and the lowest phytate content of the foods analyzed in the study. The usage of processing strategies and dietary diversification to reduce phytate content would significantly improve estimated mineral bioavailability in plant-based diets.

Fermentation of pseudocereals quinoa, canihua, and amaranth to improve mineral accessibility through degradation of phytate.

BACKGROUND: Pseudocereals are nutrient-rich grains with high mineral content but also phytate content. Phytate is a mineral absorption inhibitor. The study's aim was to evaluate phytate degradation during spontaneous fermentation and during Lactobacillus plantarum 299v® fermentation of quinoa, canihua, and amaranth grains and flours. It also aimed to evaluate the accessibility of iron, zinc, and calcium and to estimate their bioavailability before and after the fermentation of flours with starter culture. Lactic acid, pH, phytate, and mineral content were analyzed during fermentation. RESULTS: Higher phytate degradation was found during the fermentation of flours (64-93%) than during that of grains (12-51%). Results suggest that phytate degradation was mainly due to endogenous phytase activity in different pseudocereals rather than the phytase produced by added microorganisms. The addition of Lactobacillus plantarum 299v® resulted in a higher level of lactic acid (76.8-82.4 g kg-1 DM) during fermentation, and a relatively quicker reduction in pH to 4 than in spontaneous fermentation. Mineral accessibility was increased (1.7-4.6-fold) and phytate : mineral molar ratios were reduced (1.5-4.2-fold) in agreement with phytate degradation (1.8-4.2-fold) in fermented flours. The reduced molar ratios were still above the threshold value for the improved estimated mineral bioavailability of mainly iron. CONCLUSION: Fermentation proved to be effective for degrading phytate in pseudocereal flours, but less so in grains. Fermentation with Lactobacillus plantarum 299v® improved mineral accessibility and estimated bioavailability in flours. © 2019 The Authors. Journal of The Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.

Multilayer Bixin Microcapsules: The Impact of Native Carbohydrates on the Microencapsulation Efficiency and Dispersion Stability.

Bixin is a hydrophobic carotenoid present in the integument of the seeds of Bixa orellana. Microencapsulation was applied to obtain water dispersible formulations and protect the colorant against degradation. Microencapsulated systems were obtained by spray-drying a mild alkaline bixin dispersion with different encapsulating materials. The encapsulation trials were performed with and without native carbohydrates of the integument in addition to the main encapsulant. It was possible to dry dispersions with up to 10% bixin counted on total solids. All the studied systems were characterized by colorimetry, UV-vis spectroscopy, Scanning Electron Microscopy, light microscopy, turbidometric sedimentation analyses and laser light diffraction analyses. All the systems showed aqueous dispersibility but displayed differences in their transparency, UV-vis spectra and physical stability at pH 3. The results show that the native carbohydrates enhance the encapsulation efficiency of other encapsulating materials. The chemical composition of this native carbohydrate fraction shows the presence of polysaccharides containing arabinose, galactose and glucose as monomers. Starch was identified enzymatically. The native carbohydrates allowed the encapsulation of bixin in its native microcrystalline form, resulting in a multilayer structure after spray-drying. In addition, the colorant particles displayed dispersibility under acidic aqueous conditions suggesting that they are stabilized by the native carbohydrates after the microcapsules are dissolved.

Physicochemical and structural properties of starch from five Andean crops grown in Bolivia.

Three Andean grains - amaranth (Amaranthus caudatus), quinoa (Chenopodium quinoa), canihua (Chenopodium pallidicaulle) - and two Andean roots starches - achira (Canna indica), maca (Lepidium meyenii) - were studied. Physicochemical properties such as granule size, crystallinity, pasting properties among other as well as structural properties such as root-mean-square radius (rrms), weight-average molar mass (Mw) and apparent density (ρapp) were analyzed in order to evaluate the relation between them. Grains were similar in most of their characteristics as roots in their i.e. granule size, shape, type of crystallinity, Mw and rrms varied according to botanical source. The starch granules from grains were in a narrow diameter range (0.5 to 2 µm) and displayed A-type X-ray diffraction pattern (XRD). Roots starch had a wide granule diameter range (1 to 100 µm) and displayed a B-type XRD. The amylose content varied between 0 and 48% where amaranth had the lowest value and achira had the highest. Furthermore, quinoa and canihua starches had very low breakdown in pasting properties, indicating high stability during cooking. A model is proposed that relates pasting properties i.e. peak viscosity and final viscosity with ρapp, gelatinization enthalpy, granule size and amylose content.

Effect of fermentation and dry roasting on the nutritional quality and sensory attributes of quinoa.

BACKGROUND: Quinoa is a pseudocereal with relatively high content of proteins and minerals that also contains mineral inhibitors such as phytate. The aim of the present study was to evaluate lactic acid fermentation and dry roasting on the nutritional quality and sensory attributes of quinoa. Various processes were evaluated, and quinoa grains were dry-roasted, milled, and fermented, either with or without the addition of wheat phytase or activated quinoa phytase (added as back-slop starter), for 10 hr. In other processes, raw quinoa flour was fermented for 10 hr or 4 hr and dry-roasted. Hedonic sensory evaluation was then performed to evaluate the acceptability of the fermented flours prepared as porridges. RESULTS: The combined dry roasting and fermentation processes significantly (p < .05) degraded phytate between 30% and 73% from initial content. The most effective process was fermentation of raw quinoa flour followed by dry roasting, which improved the estimated zinc and iron bioavailability. Particularly, estimated zinc bioavailability improved from low (Phy:Zn 25.4, Phy·Zn:Ca 295) to moderate (Phy:Zn 7.14, Phy·Zn:Ca 81.5). Phytate degradation was mainly attributed to the activation of endogenous phytase during fermentation. Dry roasting was effective in improving the sensory attributes of the fermented quinoa flour. Porridge made with raw quinoa flour fermented for 4 hr and dry-roasted was more favorable to overall acceptability than that which was fermented for 10 hr and dry-roasted. CONCLUSION: Fermentation of quinoa flour for 4 hr followed by dry roasting was successful in improving both nutritional and sensory attributes of the final product.

Development and evaluation of methods for starch dissolution using asymmetrical flow field-flow fractionation. Part II: Dissolution of amylose.

In this paper, we investigate whether dissolution in water under autoclaving conditions (140 °C, 20 min) or in dimethyl sulfoxide, DMSO (100 °C, 1 h), is preferable for characterization of amylose. Two types of amylose, potato and maize, were dissolved either in water using an autoclave or in DMSO. On the aqueous solutions obtained, the extent of molecular dissolution of the sample (referred to as the dissolution yield) was determined by enzymatic analysis as well as the molecular properties, such as molar mass and root-mean-square radius, obtained with asymmetrical flow field-flow fractionation coupled to multi-angle light scattering and differential refractive index detection (AF4-MALS-dRI). The results showed that both dissolution methods are efficient at dissolving amylose. However, AF4-MALS-dRI analysis revealed substantial differences. Amylose aqueous solutions obtained by dissolution in DMSO were relatively stable over time, but the dissolution method in autoclave caused some degradation of the molecules, and their solutions display a high tendency to retrograde.

Phase Segregation in Individually Dried Particles Composed of Biopolymers.

Mixing of two biopolymers can results in phase separation due to their thermodynamically incompatibility under certain conditions. This phenomenon was first reported when the solution was allowed to equilibrate, but it has later been observed also as a consequence of drying. The challenges of this study were to observe phase segregation by confocal Raman microscopy and LV-SEM on dried film, individually dried particles, and spray dried particles. The influence of the solid content and the phase ratio (composition) of a HPMC/maltodextrin mixture on the localization of the ingredients in the individually dried particles was investigated. We observed that phase segregation of HPMC and maltodextrin is induced by solvent evaporation in film drying, single particle drying, as well as spray drying. The phase ratio is an important parameter that influences the localization of the HPMC-enriched phase and maltodextrin-enriched phase, i.e., to the particle surface, to the core, or in a more or less bicontinuous pattern. The drying time, affected by the solids content, was found to control the level of advancement of the phase segregation.

Development and evaluation of methods for starch dissolution using asymmetrical flow field-flow fractionation. Part I: Dissolution of amylopectin.

We have investigated methods of starch dissolution with the aim of finding an optimum method to completely dissolve starch granules to form a molecularly dissolved starch solution without degradation of the polymers. Glycogen was used as a model molecule for amylopectin, to identify the dissolution conditions under which the degradation of the polymers was limited or not present. Dissolution was performed in water with temperatures up to 200 °C, facilitated by the use of heating in an autoclave or a microwave oven, or in dimethyl sulfoxide (DMSO) at 100 °C. Waxy maize starch was chosen due to its high content of amylopectin and very low content of amylose. The degree of starch dissolution under different conditions was determined enzymatically. The effect of different dissolution conditions on the molar mass and root-mean-square radius of the polymers was determined with asymmetrical flow field-flow fractionation coupled to multi-angle light scattering and differential refractive index (AF4-MALS-dRI) detectors under aqueous conditions. The results suggest that reliable and accurate size separation and characterization of amylopectin can be obtained by dissolution of starch granules in an aqueous environment at 140 °C by autoclaving or in DMSO at 100 °C. The results also clearly show an upper limit for heat treatment of starch, above which degradation cannot be avoided.

Relating genes in the biosynthesis of the polyphenol composition of Andean colored potato collection.

The objective of this study was to evaluate total antioxidant capacity (TAC), total phenolic content (TPH), and the identification of anthocyanidin and polyphenolic compounds in 13 colored potatoes collected from the Andean region of Bolivia, and understand how the chemical composition correlated with the botanical classification and molecular characterization of genes, ans (anthocyanidin synthase) and stan1 (Solanum tuberosum anthocyanidin synthase), associated with the synthesis of anthocyanidins. The results show the existence of a limited correlation between botanical classification, based on morphological identification and polyphenol composition. No association between genetic grouping of the ans and stan genes and botanical classification was found. However, it was possible to identify a correlation between the ans gene clades and the levels of anthocyanidins as well as of other polyphenols. Thus, this result confirms the concept that potato color can be used in the search for high polyphenol potato cultivars.

Straightforward rapid spectrophotometric quantification of total cyanogenic glycosides in fresh and processed cassava products.

In this study, we extend pioneering studies and demonstrate straightforward applicability of the corrin-based chemosensor, aquacyanocobyrinic acid (ACCA), for the instantaneous detection and rapid quantification of endogenous cyanide in fresh and processed cassava roots. Hydrolytically liberated endogenous cyanide from cyanogenic glycosides (CNp) reacts with ACCA to form dicyanocobyrinic acid (DCCA), accompanied by a change of colour from orange to violet. The method was successfully tested on various cassava samples containing between 6 and 200 mg equiv. HCN/kg as verified with isonicotinate/1,3-dimethylbarbiturate as an independent method. The affinity of ACCA sensor to cyanide is high, coordination occurs fast and the colorimetric response can therefore be instantaneously monitored with spectrophotometric methods. Direct applications of the sensor without need of extensive and laborious extraction processes are demonstrated in water-extracted samples, in acid-extracted samples, and directly on juice drops. ACCA showed high precision with a standard deviation (STDV) between 0.03 and 0.06 and high accuracy (93-96%). Overall, the ACCA procedure is straightforward, safe and easily performed. In a proof-of-concept study, rapid screening of ten samples within 20 min has been tested.

Characterization of oat proteins and aggregates using asymmetric flow field-flow fractionation.

The soluble proteins and protein aggregates in Belinda oats were characterized using asymmetric flow field-flow fractionation (AF4) coupled with online UV-vis spectroscopy and multiangle light-scattering detection (MALS). Fractions from the AF4 separation were collected and further characterized by sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE). The AF4 fractogram of the oat extracts revealed three peaks which were determined to be monomeric forms of soluble proteins, globulin aggregates, and ß-glucan, respectively. The early eluting monomeric proteins ranged in molar mass (MM) between 5 and 90 kg/mol and in hydrodynamic diameter (D h) from 1.6 to 13 nm. The MM at peak maximum of the globulin aggregate peak was found to be ∼300 kg/mol and the D h was measured to be ∼20 nm. SDS-PAGE of the collected fraction across this peak revealed two bands with MM of 37 and 27 kg/mol which correspond to the α and ß subunits of globulin indicating the elution of globulin aggregates. A third peak at long retention time was determined to be ß-glucan through treatment of the oat extract with ß-glucanase and by injection of ß-glucan standards. The amount of soluble protein was measured to be 83.1 ± 2.3 wt.%, and the amount of albumin proteins was measured to be 17.6 ± 5.7 wt.% of the total protein in the oats. The results for Belinda oat extracts show that the AF4-MALS/UV platform is capable of characterizing the physicochemical properties such as MM and hydrodynamic size distribution of proteins and protein aggregates within a complicated food matrix environment and without the need to generate protein isolates.

Hydrodynamic radius determination with asymmetrical flow field-flow fractionation using decaying cross-flows. Part II. Experimental evaluation.

In this study we investigate the effect of programmed cross-flows on the error in the hydrodynamic radii (r(h)) determination with asymmetrical flow field-flow fractionation (AsFlFFF). Three different standard polystyrene particles (nominal radii of 30 and 40 and 50 nm) are fractionated with exponentially and linearly decaying cross-flows with different decay rates. Hydrodynamic radii are calculated according to retention theory including steric effects. Rapid decay is expected to give rise to systematic deviations in r(h) determination. The error in r(h) was found to be small when decay rates with half-lives longer than 6 min were used, whereas steeper decays could give rise to errors as high as 16% of the particle size. The error is often explained in terms of secondary relaxation. However, comparisons show that experimental errors are significantly larger than what would be expected due to secondary relaxation, suggesting that other factors also have to be considered in order to fully understand deviations for rapidly decaying cross-flow.

Hydrodynamic radius determination with asymmetrical flow field-flow fractionation using decaying cross-flows. Part I. A theoretical approach.

Direct determination of hydrodynamic radius from retention time is an advantage of the field-flow fractionation techniques. However, this is not always completely straight forward since non-idealities exist and assumptions have been made in deriving the retention equations. In this study we investigate the effect on accuracy from two factors: (1) level of sophistication of the equations used to determine channel height from a calibration experiment and (2) the influence of secondary relaxation on the accuracy of hydrodynamic radius determination. A new improved technique for estimating the channel height from calibration experiments is suggested. It is concluded that severe systematic error can arise if the most common channel height equations are used and an alternative more rigorous approach is described. For secondary relaxation it is concluded that this effect increases with the cross-flow decay rate. The secondary relaxation effect is quantified for different conditions. This is part one of two. In the second part the determination of hydrodynamic radius are evaluated experimentally under similar conditions.