Microwaved-Assisted Synthesis of Starch-Based Biopolymer Membranes for Novel Green Electrochemical Energy Storage Devices.

The investigated starch biopolymer membrane was found to be a sustainable alternative to currently reported and used separators due to its properties, which were evaluated using physicochemical characterization. The molecular dynamics of the biomembrane were analyzed using low-field nuclear magnetic resonance (LF NMR) as well as Raman and infrared spectroscopy, which proved that the chemical composition of the obtained membrane did not degrade during microwave-assisted polymerization. Easily and cheaply prepared through microwave-assisted polymerization, the starch membrane was successfully used as a biodegradable membrane separating the positive and negative electrodes in electric double-layer capacitors (EDLCs). The obtained results for the electrochemical characterization via cyclic voltammetry (CV), galvanostatic charge with potential limitation (GCPL), and electrochemical impedance spectroscopy (EIS) show a capacitance of 30 F g-1 and a resistance of 2 Ohms; moreover, the longevity of the EDLC during electrochemical floating exceeded more than 200 h or a cyclic ability of 50,000 cycles. Furthermore, due to the flexibility of the membrane, it can be easily used in novel, flexible energy storage systems. This proves that this novel biomembrane can be a significant step toward ecologically friendly energy storage devices and could be considered a cheaper alternative to currently used materials, which cannot easily biodegrade over time in comparison to biopolymers.

Chemical Characteristics and Thermal Oxidative Stability of Novel Cold-Pressed Oil Blends: GC, LF NMR, and DSC Studies.

Plant oils contain a high content of unsaturated fatty acids. Studies of food products have revealed a considerable disproportion in the ratio of ω6 to ω3. This article presents information on the healthful qualities of eight new oil blends that contain a beneficial proportion of ω6 to ω3 fatty acids (5:1), as well as their degradation during heating at 170 and 200 °C. The fatty acid profile was analyzed by gas chromatography (GC), content of polar compounds and polymers of triacylglycerols by liquid chromatography (LC), water content was measured by the Karl Fischer method, and oxidative stability was measured by differential scanning calorimetry (DSC) and low-field nuclear magnetic resonance (LF NMR) methods. The results showed that during heating, the polar fraction content increased in samples heated at both analyzed temperatures compared to unheated oils. This was mainly due to the polymerization of triacylglycerols forming dimers. In some samples that were heated, particularly those heated to 200 °C, trimers were detected, however, even with the changes that were observed, the polar fraction content of the blends did not go beyond the limit. Despite the high content of unsaturated fatty acids, the analyzed blends of oils are characterized by high oxidative stability, confirmed by thermoanalytical and nuclear magnetic resonance methods. The high nutritional value as well as the oxidative stability of the developed oil blends allow them to be used in the production of food, in particular products that ensure an adequate supply of ω3 fatty acids.

Effect of Flaxseed Oil Cake Extract on the Microbial Quality, Texture and Shelf Life of Gluten-Free Bread.

Extending the shelf life of gluten-free bread (GFB) is a challenge. Mainly due to the ingredients used and their characteristics, GFB has numerous drawbacks such as unsatisfactory texture and rapid staling beyond a low nutritional value. In the present study, flaxseed oil cake extract (FOCE) was used to replace water (25-100%) in GFB formulations in order to test FOCE's potential to reduce GFB staling and extend microbial stability. Texture (TPA test), water activity (LF NMR), acidity (pH measurements) and microbiological quality of GFBs were tested. Moreover, the content of a lignan with broad health-promoting potential, secoisolariciresinol diglucoside (SDG), in GFB with FOCE was analyzed. The results showed that the use of FOCE enriched experimental GFB in valuable SDG (217-525 µg/100 g DM) while not causing adverse microbiological changes. A moderate level (25-50%) of FOCE did not change the main texture parameters of GFB stored for 72 h, the quality of which was comparable to control bread without FOCE. Meanwhile, higher proportions of FOCE (75-100% of water replacement) shortened GFB shelf life as determined by water activity and texture profile, suggesting that GFB with FOCE should be consumed fresh. To summarize, FOCE at moderate levels can add value to GFBs without causing a drop in quality, while still fitting in with the idea of zero waste and the circular economy.

Chemical Modifications of Normal and Waxy Potato Starches Affect Functional Properties of Aerogels.

Aerogels are of increasing interest because of their exceptionally large surface area, porous structure, and low weight. Despite the significant increase in interest in the subject of starch-based aerogels, the number of detailed studies is rather scarce, which is especially evident in the case of chemically modified derivatives. Therefore, the study aims to evaluate the physicochemical properties of aerogels from chemically modified potato starch preparations (E 1422 and E 1450) obtained both from normal and waxy starches. Aerogels were prepared through the retrogradation of starch pastes followed by the gradual replacement of water with ethyl alcohol. The obtained preparations were characterized in terms of their bulk density, oil-binding capacity, as well as the texture and rheological properties of the formed pastes. Moreover, their usefulness was evaluated in an emulsion system employing rheological and low-field NMR methods. The obtained aerogels were characterized by a lower bulk density of 0.18-0.59 g/cm3 and 5.4-6.6 times higher oil-binding capacity compared to native potato starch. The chemical modification of starch helped to further alter the functional properties of the obtained aerogels, making them more effective oil binders, emulsifiers, and stabilizers (increasing the stability from 55 to 90%), which was especially evident for E 1450 preparation. Amylose content improved the aerogel properties, as waxy preparations were characterized by worse functional properties with the only exception of improved thickening ability. The most beneficial properties for the preparation of emulsions were observed for the aerogel obtained based on E 1450 normal potato starch.

The Effect of Packaging Methods, Storage Time and the Fortification of Poultry Sausages with Fish Oil and Microencapsulated Fish Oil on Their Rheological and Water-Binding Properties.

The aim of the study was to investigate how liquid fish oil and microencapsulated oil additives influenced the rheological characteristics and the dynamics of water binding in vacuum-packed (VP) and modified-atmosphere-packed (MAP) poultry sausages during 21-day storage. In contrast to the control sample, the sausages enriched with microencapsulated fish oil (MC) were characterised by the greatest ability to accumulate deformation energy. The elastic properties of all sausage variants increased significantly in the subsequent storage periods, whereas the dynamic viscosity of the samples tended to decrease. This phenomenon was confirmed by the gradual reduction of water activity (Aw) in all sausages in the subsequent storage periods. The packaging method influenced the dynamics of water binding in an oil-additive-form-dependent manner. During the storage of the VP and MAP sausages, in samples with the fish oil additive the T1 value tended to increase while the Aw decreased. The T1 value in the MAP MC sample was similar. The FO additive resulted in greater mobility of both proton fractions in the MAP samples than in the VP samples. There were inverse relationships observed in the MC samples. The NMR tests showed that the VP samples with the MC additive were slightly better quality than the other samples.

Pasta with Kiwiberry (Actinidia arguta): Effect on Structure, Quality, Consumer Acceptance, and Changes in Bioactivity during Thermal Treatment.

In this study, kiwiberry lyophilizate (KBL) was incorporated into pasta at different levels (5%, 10%, and 15% w/w). Kiwiberry fruits' characteristics (ascorbic acid, carotenoids, phenolic compounds, and antioxidant activity determination) as well as physical (cooking properties, color, microscopic structure determination, texture, and water molecular dynamics analysis by low-field NMR) and chemical analyses (proximate composition phenolic compounds composition and antioxidant activity) of KBL-enriched pasta were investigated. The replacement of semolina with KBL in the production of pasta significantly changed its culinary properties. Results showed that the addition of KBL leads to a reduction in optimal cooking time and cooking weight (47.6% and 37.3%, respectively). Additionally, a significant effect of the KBL incorporation on the color of both fresh and cooked pasta was observed. A significant reduction in the L* value for fresh (27.8%) and cooked (20.2%) pasta was found. The KBL-enriched pasta had a different surface microstructure than the control pasta and reduced firmness (on average 44.7%). Low-field NMR results have confirmed that the ingredients in kiwiberry fruit can bind the water available in fresh pasta. The heat treatment resulted in increasing the availability of phenolic compounds and the antioxidant activity (64.7%) of cooked pasta. Sensory evaluation scores showed that the use of 5-10% of the KBL additive could be successfully accepted by consumers.

Polymer-Solvent Interactions in Modified Starches Pastes-Electrokinetic, Dynamic Light Scattering, Rheological and Low Field Nuclear Magnetic Resonance Approach.

Starch paste is a very complex dispersion that cannot be clearly classified as a solution, colloid or suspension and many factors affects its properties. As these ambiguities constitute a barrier to technological development, the aim of this study was to investigate the interaction of starch macromolecules with water by analysing the results of rheological properties, low field nuclear magnetic resonance (LF NMR), dynamic light scattering (DLS) and ζ potential analyses. Starch pastes with a concentration of 1%, prepared with distilled water and buffered to pH values of 2.5, 7.0 and 9.5 were analysed. It was proved that the pH buffering substantially decreased the values of consistency index but the pH value itself was not significant. LF NMR studies indicated that the dissolution of starch in water resulted in a reduction in spin-lattice as well as spin-spin relaxation times. Moreover, changes in relaxation times followed the patterns observed in rheological studies. Electrokinetic and DLS analyses showed that potential values are primarily influenced by the properties of the starches themselves and, to a lesser extent, by the environmental conditions. The conducted research also showed complementarity and, to some extent, substitutability of the applied research methods as well as exclusion chromatography (a method not used in this work).

Influence of Xanthan Gum Addition on the Short- and Long-Term Retrogradation of Corn Starches of Various Amylose Content.

Starch retrogradation is a complex process and in most food products is undesirable. Knowing and understanding the mechanisms and factors that influence this process may become the key to a better and innovative approach to food design. In this paper, we investigated the effect of 0%, 0.05% and 0.20% (w/w) xanthan gum (XG) addition on the short- and long-term retrogradation of 4%, 5% and 6% corn starch gels, depending on the amylose/amylopectin ratio in the starch. The changes were monitored throughout 90 days. The pasting characteristics of blends, rheological and texture analyses, as well as syneresis, revealed that XG stabilizes the starch in the short term, but it does not inhibit retrogradation caused by amylopectin. After 30 days of storage, the destabilization of the starch-hydrocolloid mixture was observed. Based on the obtained results, a probable mechanism for the retrogradation of corn starch process in the presence of xanthan gum was proposed.

The Process of Pasting and Gelling Modified Potato Starch with LF-NMR.

Currently, society expects convenience food, which is healthy, safe, and easy to prepare and eat in all conditions. On account of the increasing popularity of modified potato starch in food industry and its increasing scope of use, this study focused on improving the physical modification of native starch with temperature changes. As a result, it was found that the suggested method of starch modification with the use of microwave power of 150 W/h had an impact on the change in starch granules. The LF-NMR method determined the whole range of temperatures in which the creation of a starch polymer network occurs. Therefore, the applied LF-NMR technique is a highly promising, noninvasive physical method, which allows obtaining a better-quality structure of potato starch gels.

Water Behavior of Aerogels Obtained from Chemically Modified Potato Starches during Hydration.

Aerogels are highly porous materials that are prepared by removing water held within a hydrogel in a manner that maintains the three-dimensional structure of the gel. Recently, there has been much interest in the preparation of aerogels from biopolymers, including starch. The applicability of native starches in the food industry is partially limited; therefore, the functional properties of starch are often improved by means of physical and/or chemical modification. The aim of the work was the analysis of molecular dynamics and the transport of water in aerogels obtained from native and chemically modified potato starches of the normal and waxy variety. Chemical modification with OSA (E 1450) as well as cross-linking with adipic anhydrite and acetylation (E 1422) had no significant impact on the hydration of potato starch aerogels as well as equilibrium water activity. The introduction of chemical moieties into starch macromolecules led to the improved binding of water by the biopolymer matrix; this was especially evident in the case of waxy starch derivatives. A increase in the amylopectin-to-amylose ratio of starch used for production of aerogels resulted in a decrease of equilibrium water activity along with spin-lattice relaxation time.

Whey Proteins as a Potential Co-Surfactant with Aesculus hippocastanum L. as a Stabilizer in Nanoemulsions Derived from Hempseed Oil.

The use of natural surfactants including plant extracts, plant hydrocolloids and proteins in nanoemulsion systems has received commercial interest due to demonstrated safety of use and potential health benefits of plant products. In this study, a whey protein isolate (WPI) from a byproduct of cheese production was used to stabilize a nanoemulsion formulation that contained hempseed oil and the Aesculus hippocastanum L. extract (AHE). A Box-Behnken experimental design was used to set the formulation criteria and the optimal nanoemulsion conditions, used subsequently in follow-up experiments that measured specifically emulsion droplet size distribution, stability tests and visual quality. Regression analysis showed that the concentration of HSO and the interaction between HSO and the WPI were the most significant factors affecting the emulsion polydispersity index and droplet size (nm) (p < 0.05). Rheological tests, Fourier transform infrared spectroscopy (FTIR) analysis and L*a*b* color parameters were also taken to characterize the physicochemical properties of the emulsions. Emulsion systems with a higher concentration of the AHE had a potential metabolic activity up to 84% in a microbiological assay. It can be concluded from our results that the nanoemulsion system described herein is a safe and stable formulation with potential biological activity and health benefits that complement its use in the food industry.

Low-Field NMR Study of Shortcake Biscuits with Cricket Powder, and Their Nutritional and Physical Characteristics.

The growing human population renders challenges for the future supply of food products with high nutritional value. Here, we enhanced the functional and nutritional value of biscuits, a popular sweet snack, by replacing the wheat flour with 2%, 6%, or 10% (w/w) cricket powder. Consumer acceptance ratings for reference and 2% augmented cookies were comparable, whereas the higher levels of enhancement received inferior consumer scores. This relatively small change in biscuit recipe provided significant and nutritionally desirable enhancements in the biscuits, observed in a series of analyses. An increase in the protein content was observed, including essential amino acids, as well as minerals and fat. This conversion also affected the physical properties of the biscuits, including hardness, and water molecular dynamics measured by 1H NMR. Cricket powder-augmented biscuits join the line of enhanced, functionally superior food products. This and similar food augmentation provide a viable scenario to meet the human food demands in the future.

Water Behavior of Emulsions Stabilized by Modified Potato Starch.

Starch is a widely known and used emulsion stabilizer. In order to improve its properties, various types of modifications are made that change its ability to emulsify and stabilize. This paper describes the analysis of the molecular dynamics of water using low-field nuclear magnetic resonance (LF NMR) in oil-in-water emulsions obtained with the use of physically or chemically modified potato starch. The analysis of changes in spin-spin and spin-lattice relaxation times depending on the temperature allowed the activation energy value of water molecules in the analyzed emulsions to be determined. It has been shown that the presence of starch influences the values of spin-lattice T1 and spin-spin T2 relaxation times, both in the water and the oil phase, and the observed changes largely depended on the type of starch modification. Both types of analyzed starches also differently influenced the energy of activation of rotational movements of water molecules. On the basis of the analyses carried out with the use of LF NMR, it can be concluded that physically modified starch acts not only as a stabilizer, but also as an emulsifier, while acetylated starch does not exhibit good emulsifying properties.

Multidisciplinary Studies of Folk Medicine "Five Thieves' Oil" (Olejek Pieciu Zlodziei) Components.

To meet the growing interest in natural antibacterial agents, we evaluated the physicochemical and biological properties of the folk medicine known as "five thieves' oil" (Polish name: olejek pieciu zlodziei). Five thieves' oil consists of a mixture of five oils: rosemary, lemon, clove, eucalyptus, and cinnamon. In this study, we performed gas chromatography, FTIR, and UV-vis spectroscopic analysis, as well as L-a-b color tests, contact angle determination, and surface tension determination. To verify its antibacterial activity, the metabolic activity and changes in cell membrane permeability of bacteria of the genus Pseudomonas were studied. As a result, it was found that among the constituent oils, the oils of clove and cinnamon were the least volatile and, at the same time, had the strongest antibacterial activity. However, a mix of all the oils also showed comparable activity, which was even more pronounced for the oils after 4 weeks of aging. This effect can be linked to the high content of terpene derivatives such as eugenol and cinnamaldehyde, which can cause changes in bacterial membrane permeability, affecting cell activity and survival. This study is the first to characterize the constituents of the popular folk medicine five thieves' oil, confirming and explaining its strong antibacterial activity, thus constituting a significant contribution to contemporary health education.

LF NMR spectroscopy analysis of water dynamics and texture of Gluten-Free bread with cricket powder during storage.

The paper presents the effect of replacing starch (at 2%, 6% and 10%) with cricket powder (CP) on the water behavior studied by the 1H NMR method, as well as the texture of gluten-free bread during 6-day storage. It was noticed that the bread crumb containing CP has lower water transport rate than the control bread crumb, while concluding that 2% CP stabilizes water transport throughout the entire staling time range. The NMR analyzes showed that the initial T21 values are the higher, the more starch has been replaced with the CP, however, after 6 days of storage, all tested samples are characterized by similar values of the T21 parameter. A decrease in long component of spin-spin relaxation time T22 during storage was also observed. It has been noted that the replacement of starch to 2% and 6% CP causes an increase in the molecular dynamics of water. The less starch present, the greater the potential for bulk molecules to move. The observed changes at the molecular level resulted in macroscopic changes in the texture of the bread. After analyzing the hardness parameter of the tested breads, it was found that on the day of baking, bread without the addition of CP had significantly higher values of this parameter than breads with CP. For the sample without CP, the highest increase in total hardness change (123.93%) was noted during storage, which indicates the fastest texture change process. Based on the results obtained, it can be concluded that the use of cricket powder to enrich gluten-free bread can not only improve the nutritional value, but also effectively delay the process of bread staling.

Fluorescent Submicron-Sized Poly(heptafluoro-n-butyl methacrylate) Particles with Long-Term Stability.

Fluorescent submicron particles of fluorinated methacrylate (HFMBA) with long-term stability have been synthesized and characterized with regard to their potential applications. Rhodamine B (RBITC) isothiocyanate was used as the fluorescent component. The core-shell structure of the particles effectively protected the dye against bleaching. HFBMA nanoparticle (NP) stability was confirmed after seven years of storage. Only slight differences were found in the polydispersity index (pdi) from 0.002 to 0.010. Particle size measurements were carried out using dynamic light scattering (DLS), nanoparticle tracking (NTA), and fluorescence correlation spectroscopy (FCS). The hydrodynamic diameter evaluated by different methods were in good agreement, respectively: 184-550 nm, 218-579 nm, and 236-508 nm. Particle and core morphology was estimated by using scanning and transmission electron microscopy (SEM and TEM). The ability to recognize particles in 3D as a reference sample in biological media has been confirmed by epifluorescence optical microscopy, confocal laser scanning microscopy, and super-resolution confocal microscopy (STED).

Molecular Analysis of Retrogradation of Corn Starches.

Changes of the molecular dynamics of water in 5% corn starch pastes and 5% systems composed of starch and non-starchy hydrocolloid were studied during short and long term retrogradation. Low Field NMR was used to record mean correlation times (τc) of water molecules. This molecular parameter reflects the rotation of water molecules within the network of paste. Starches of different amylose and amylopectin content were selected for this study. Comparison of the changes of τc shows how particular polymers bind water molecules. During 90 days of storage, over 50% increase in mean correlation time was recorded in pastes of starches with high amylose content. This suggests that the formation of polymeric network is controlled by amylose to which water is binding. Amylopectin was found to influence the mobility of water in the pastes to a lesser extent with changes in mean correlation times of approximately 10-15% over 90 days. On retrogradation, amylopectin, Arabic and xanthan gums hindered the formation of solid phase structures. Guar gum evoked an increase in mean correlation times of approximately 40-50% during the prolonged process of changes of the molecular dynamics of water. This indicates continued expansion of the polymeric network. Mean correlation time available from spin-lattice and spin-spin relaxation times can be useful in the analysis of the rotational vibrations of the water molecules in biopolymeric structures.

Gluten-Free Bread with Cricket Powder-Mechanical Properties and Molecular Water Dynamics in Dough and Ready Product.

Published data indicate that cricket powder (CP) is a good source of not only protein, fat and fiber, but also minerals. Due to the fact that this product naturally does not contain gluten, it is an interesting addition to the enrichment of gluten-free foods. This paper is a report on the results of starch substitution with CP (at 2%, 6% and 10%) on the properties of dough and bread. The rheology of dough and the texture of the final product were studied. While the changes caused in the dough by the introduction of CP were not pronounced, the bread obtained from it was characterized by significantly increased hardness and improved consistency. Analyses of water behavior at the molecular level with the use of 1H Nuclear Magnetic Resonance (NMR) indicated that CP altered both the bound and bulk water fractions. Moreover, examination of water activity revealed a decreased rate of water transport in samples of bread that contained CP. These results indicate improved availability of water to the biopolymers of bread, which likely plays a role in shaping the textural properties of the product.

Kinetic models of quality parameters of spreadable processed Gouda cheese during storage.

The aim of the study was to prepare mathematical models based on the Arrhenius equation as predictive tools for the assessment of changes in quality parameters during the storage of spreadable Gouda cheese at temperatures of 8, 20 and 30 °C. The activation energy value and the chemical reaction rate constant enabled the construction of kinetic models, which helped to estimate the direction and rate of changes. Moreover, the activation energy (Ea) of the quality parameters was used to determine the sequence of their vulnerability during storage. The value of activation energy corresponding to temperature changes resulted in the following order of susceptibility of the quality parameters: ΔC > ΔE ≈ water activity > texture parameters > pH > colour > sensory parameters > rheological parameters. The research showed limited applicability of the mathematical models for estimation of quality parameters referring to spreadable processed Gouda cheese.

A novel method of recognizing liquefied honey.

The content of glucose, fructose, sucrose, maltose and water were determined for multiflorous honey of Great Poland. The measurements were carried out for different fractions of honey and also for the liquefied honey at 40 °C. Water activity and pH were both determined for all samples. A new method of recognizing liquefied honey is proposed based on the water influence on pH and the monosaccharides and disaccharides contents. The simple function of quadratic polynomial enabled to reveal the different character of the liquefied honey. The electrical conductivity behavior of different dry matter samples of honey are presented in the wide range of temperature. The proton spin-lattice relaxation measurements were recorded for the crystalline fraction in the magnetic field range covering the proton Larmor frequencies from 0.01 to 25 MHz and in the wide range of temperature. Heating the honey at 30 °C results in the irreversible molecular structure changes.