Several studies have demonstrated the use of terahertz waves to estimate mass diffusion coefficients under transient conditions. Monitoring transient water content is recognized as a key parameter in many drying processes (e.g., wood, paper, etc.). However, accurate control of this physical quantity remains essential to ensure product quality and, in the case of food products, to extend shelf life. In this study, terahertz waves were employed to locally measure the water content in a cereal-based product, using a muffin as a case study. To characterize the spatial distribution of water within the product, the muffin was sliced into sections of equal thickness and scanned using a terahertz line camera. By comparing the transmitted signals obtained from the wet and dry samples, the local water content of each slice was determined. Stacking the resulting measurement planes provides an overall water-content distribution within the muffin.

The ability of proteins to foam is an important functionality in aerated food products. The functionalities of animal proteins over plant proteins are undeniable. However, plant-based ingredients have now became common substitutes. Among the available plant protein sources, yellow peas have been widely studied. This paper focuses on the functionalities of a pea protein concentrate (PPC) obtained after simpler and less damaging processes than those for isolates.Pea protein concentrate dispersions underwent ultrasounds, heating, or enzymatic hydrolysis. Physical treatments did not affect pea protein’s structure, unlike enzymatic hydrolysis, which significantly altered the molecular size distribution. Enzymatic hydrolysis emerged as the most effective pathway for enhancing PPC foamability. Foams produced from concentrated hydrolyzed PPC (HYD PPC) dispersions were compared to whole egg foams. Interestingly, HYD PPC foams exhibited solid-like behavior, while whole egg foams displayed flowing behavior and lower stability over time. The solid fraction and the presence of polysaccharides in HYD PPC dispersions prevented drainage and coalescence in HYD PPC foams, ensuring excellent stability. Interfacial behavior differed in terms of kinetics of adsorption at the air/water interface between HYD PPC and whole egg proteins, yet both formed interfacial films with high viscoelastic properties.

Lipases were used in this study with rapeseed oil in order to generate insitu mono- and di-glycerides of fatty acids (MDGs) and free fatty acids (FFAs). Those compounds are interesting to preserve softness in sponge cakes and largely, this strategy can be used as a clean-label approach to replace some added synthetic additives. Modifying rapeseed oil with such enzymes can only be made through an emulsification. With this biphasic system, the modified oil can be easily removed and used for food application whereas the aqueous phase (containing lipase) can be re-emulsified with fresh oil. In this study, we investigated the possibility of recycling the lipase and followed the overall activity up to 25 cycles thanks to Acid Value and 13C NMR as main indicators for molecular determination in the oil phase as well as 1H NMR for glycerol accumulation in the aqueous phase. A decrease of triglycerides conversion (-56 %) as well as a change in the selectivity (+50 % of FFAs with a slight change in MDGs production) was obtained and may be explained by an accumulation of glycerol at the interface. Nevertheless, when modified oils were used as ingredient in sponge cake fabrication and compared to rapeseed oil, the softness was preserved during a storage period of 3 months, regardless of the number of cycles (+104 % in hardness for the control product and a range of +26-45 % when oils are preferably used). Thus, recycling lipases can be considered as an economically valuable strategy.

Omega-3 fatty acid supplements, such as fish oil and plant-based oils, have gained popularity because of their potential health benefits. However, the quality and composition of these supplements can vary widely, particularly in terms of the two main forms of omega-3 fatty acids: triacylglycerols (TAGs) and ethyl esters (EEs). TAGs are the natural form found in fish oil but are prone to oxidation, whereas EEs are more stable but less well absorbed by the body. Differentiating between these forms is crucial for assessing the efficacy and tolerance of omega-3 supplements. This article describes a novel approach to differentiate between TAG and EE forms of omega-3 fatty acids in dietary supplements, utilizing a 60-MHz benchtop nuclear magnetic resonance (NMR) spectrometer. The proposed method using 1H and 1H-1H COSY NMR provides a quick and accurate approach to screen the forms of omega-3 fatty acids and evaluate their ratios. The presence of diacylglycerol (DAGs) in some supplements was also highlighted by this method and adds some information about the process used (i.e., esterification/enrichment). The affordability and user-friendliness of benchtop NMR equipment make this method feasible for food processing companies or quality control laboratories. In this study, 24 oil supplements were analyzed using NMR analysis in order to demonstrate the potential of this method for the differentiation of TAG and EE forms in omega-3 supplements.

We investigated the possibility to use rapeseed as a main oil in ice cream formulations by changing its functionality when using different kinds of lipases. Through a 24 h-emulsification and a centrifugation, the modified oils were further used as functional ingredients. All lipolysis was first assessed as a function of time by 13C NMR, where triglycerides consumption and the formation of low-molecular polar lipids (LMPL: monoacylglycerol and free fatty acids, FFAs) were selectively identified and compared. The more the FFAs, the sooner the crystallization (from -55 to -10 °C) and the later the melting temperatures (from -17 to 6 °C) measured by differential scanning calorimetry. These modifications were exploited in ice cream formulations with a significant impact on overall hardness (range of 60-216 N) and flowing during defrosting (from 1.29 to 0.35g/min). The global behavior of products can be controlled by the composition of LMPL within oil.

Mono- and diglycerides of fatty acids (MDGs) are commonly used in the production of sponge cakes due to their ability to form inclusion complexes with amylose, which prevents staling. They are considered as food additives and have to be mentioned on the ingredient list. The aim of this study was to use an enzymatic strategy in order to generate in situ mono- and diglycerides of fatty acids, starting from rapeseed oil and a non-GMO lipase through emulsification. Reaction products were first characterized by Gas Chromatography (GC). Proton Nuclear Magnetic Resonance (H-1 NMR) was employed as an additional technique to qualify and selectively identify the monoglyceride isomers. After 2 h of lipolysis, a high amount of MDGs was reached. Beyond this point, a continuous decrease was observed until 24 h. When used in total substitution of rapeseed oil, modified oils (2 h or 24 h) impact negatively the structure of cakes and have to be diluted before use. The structure and the softness of the products were characterized and followed up to 6 months. The best results were obtained with a 24-h enzymatic reaction and by diluting between 5 and 25 g/100 g in unmodified rapeseed oil.

Commercial oleogelators rich in monoglycerides (MGs) are complex mixtures of acylglycerides with variable gelling properties, depending on the oil used and their concentration. In this study we developed a chemometric approach to identify the key parameters involved in gelling process. Analytical parameters have been defined, using GC and NMR analysis to identify fatty acids and acylglycerides composing the mixtures. Specific acylglyceride families and compound ratios were calculated to streamline the analytical results. To determine the key analytical parameters, artificial neural networks were used in a QSPR study related to the gelling properties measured by rheology through oscillatory experiments. At low oleogelator concentrations, the MGs especially rich in C16:0 and the ratio of specific isomers both have a positive influence on G'. For high oleogelator concentrations, C18:0-rich acylglycerides and unsaturated/saturated fatty acid ratios have a positive influence on G'. Conversely, at low concentrations, C18:0-rich acylglycerides show a lesser effect on G'

The texturing properties of mercerized cellulose dispersed in rapeseed oil without any prior thermal treatment were investigated as a function of botanical origin, cellulose content, mass fraction and fiber size through a molecular analysis of samples, macroscopic/microscopic observations and rheological experiments (continuous and oscillatory shear flows). A solid-like behavior of dispersions was demonstrated for a minimum cellulose content of about 60wt% in the vegetal powder. The oleogelation efficiency increases with the mass fraction of powder in oil and the maximum size of cellulose fibers as a result of weak attractive interactions and fiber entanglement giving rise to a network entrapping the liquid phase. An innovative strategy using a 30wt% dispersion of bamboo fibers in rapeseed oil was finally used to produce in a conch a chocolate spread with a high thermal stability at 38°C and healthier nutritional qualities compared to an equivalent product prepared with palm oil.

This work investigates the structure and behavior of model oil-in-water chocolate ganaches by comparing two systems differing in the nature of the dispersed (fat) phase: cocoa butter and cocoa mass (mix of cocoa butter and fibers). Significant differences regarding the textural properties and stability were evidenced. Concentrated liquid emulsions made with cocoa butter had a thick and homogeneous macroscopic aspect. Upon cooling, fat crystallization produced partial coalescence and the emulsions became solid. With molten cocoa mass, a homogeneous aspect was observed until 50 g/100 g of dispersed phase and a grainy texture was obtained at larger fractions. This textural transition was interpreted as being due to a jamming transition. Both conventional and fluorescence microscopy revealed that cocoa fibers were transferred from the fat phase to the aqueous phase and were partially anchored to the interfaces. Upon cooling, cocoa fibers acted as a physical barrier that limited the extent of partial coalescence.

This study deals with the fabrication of inclusion complexes starting from a cross coupling of seven helical polysaccharides (host) and six flavouring agents (guest). Neither of the substrates is considered as an emulsifier when studied alone. Due to a complexation mechanism, the presence of intermolecular hydrogen bonds between substrates was highlighted by infra-red spectroscopy and 13C NMR. In addition, depending on the polysaccharide used, the guest molecule could be preferentially located either inside or in the interstitial spaces of the helix. In a comparison between raw substrates, the inclusion complexes obtained presented the unique interfacial activity of decreasing surface tension values (γ) and, in some cases, their behaviour in water was similar to that of regular emulsifiers due to the presence of a critical aggregation concentration (CAC). Substrate concentrations and the ratios between them were the main parameters investigated in this study, which focused on the two inclusion complexes: vanillin/amylose and vanillin/ι-carrageenan. The first decreased γ values by as much as 53 mN/m with a double transition, whereas the second could cause γ fall to 36 mN/m with a regular break. In addition, these systems were able to stabilize foams for up to 60 min, which confirmed their unique emulsifying properties.

Estrogenic isoflavones were found, in the 1940s, to disrupt ewe reproduction and were identified in soy-consumers' urine in 1982. This led to controversy about their safety, often supported by current Asian diet measurements, but not by historical data. Traditional Asian recipes of soy were tested while assaying soy glycosilated isoflavones. As these compounds are water-soluble, their concentration is reduced by soaking. Pre-cooking or simmering time-dependently reduces the isoflavone:protein ratio in Tofu. Cooking soy-juice for 15 or 60min decreases the isoflavone:protein ratios in Tofu from 6.90 to 3.57 and 1.80, respectively (p<0.001). Traditional Tempeh contains only 18.07% of the original soybean isoflavones (p<0.001). Soy-juice isoflavones were reduced by ultra-filtration (6.54 vs 1.24 isoflavone:protein; p<0.001). Soy-protein and isoflavones are dissociated by water rinsing and prolonged cooking, but these have no equivalent in modern processes. As regards human health, a precise definition of the safety level of isoflavone intake requires additional studies.

The incorporation of air in vegetable oils is highly sought after as it allows reducing the total fat content, while providing a light and pleasant texture. To meet consumers' requirements, nonaqueous foams must remain kinetically stable for several months and must withstand large deformations and flows. In this paper, we describe the fabrication of air-in-oil foams of outstanding stability, both at rest and under flow, based on the use of crystallizable surfactants (mixture of mono- and diglycerides). The air volume fraction is close to 55%, irrespective of the surfactant concentration. The air bubbles are protected against coalescence and Ostwald ripening by a dense layer of crystals. Moreover, the firmness of the surfactant crystal network formed in the oil bulk is large enough to hinder buoyancy driven phenomena. Finally, we demonstrate that the oil foams can be dispersed in an aqueous phase containing hydrocolloids to form a novel type of material: air-in-oil-in-water (A/O/W) emulsions.

We describe a gelation process based on the osmotically driven water flux between the two aqueous compartments of double emulsions. We first prepare fluid water-in-oil-in-water (W/O/W) double emulsions whose external aqueous phase contains hydrocolloids and/or proteins at moderate concentration. The initial osmotic pressure in the innermost droplets is considerably larger than that in the external phase. An inward water transfer (swelling) is thus likely to occur in order to restore osmotic equilibrium. In the initial state, the globules are large and so the transfer is slow because of the limited exchange surface area. The emulsions are then submitted to a short and intense shear that provokes globule breakup, in order to increase the rate of water diffusion. As a consequence, the initially fluid materials undergo a sudden rheological transition. During that process, the hydrocolloids and/or proteins are concentrated in the continuous phase until a point that a gel is formed. The final rheological properties can be tuned from weak to strong gels depending on the initial composition. The inner droplet fraction strongly increases during the swelling process and droplet–globule coalescence occurs above a critical volume fraction that determines the maximum swelling capacity and thus final state of the system. The proposed approach demonstrates a simple, yet versatile and adaptable solution for making texturized emulsions with reduced fat content and limited amount of hydrocolloids/proteins.

The use of agricultural resources for industrial purposes will undoubtly be one of the major challenges of the 21 st century. Organic biosynthons used in chemistry should progressively replace those coming from fossil fuels. Our work on dispersions of fatty acids and hydroxylated derivatives forms part of these efforts in that it seeks to demonstrate the potential contribution of fatty acids (which may be extracted from plants) as a new class of surface active agents. Dispersions of fatty acid and their hydroxyl derivatives are thus studied in solution in order to generate a new class of surface active agents for foaming and emulsifying properties.

Herein we show that glycerol can be considered as a promising cheap and green solvent for the regioselective beta,beta-diarylation of alkenes. Whereas this reaction is generally catalyzed under an inert atmosphere by expensive phosphine or carbene-palladium complexes, we show here that the diarylation of alkenes can be conveniently achieved in glycerol in the presence of air-stable palladium nanoparticles. These palladium nanoparticles were stabilized over a sugar-based surfactant derived from biomass. By an adjustment of the reaction temperature, we were able to control the mono-and diarylation step of alkenes, thus offering a convenient route to unsymmetrical diarylated alkenes. At the end of the reaction, the diarylated alkenes were cleanly and selectively extracted from the glycerol-palladium catalytic phase using supercritical carbon dioxide, thus affording a convenient purification work-up. Within the framework of green chemistry, this work combines (i) catalysis in a cheap, safe and sustainable medium, (ii) easily made and air-stable palladium nanoparticles as the catalyst, and (iii) a clean and selective extraction of the reaction products with supercritical carbon dioxide.

A new family of antioxidant ion-pair surfactants was developed by acid-base association of a fatty amine (C12 or C16) with caffeic acid, a natural antioxidant molecule. The amphiphilic molecules obtained, spontaneously formed stable vesicles in water with hydrodynamic diameters around 230 nm. Moreover, as shown by a surface tension study, they presented a phase transition from micelles to vesicles. The maintenance of the antioxidant properties of both caffeate ion-pair surfactants was confirmed by the DPPH test. The amphiphilic properties associated with the antioxidant ability of these new caffeates were used to protect complexed DNA by cationic surfactant (CTAB) from photooxidative cleavage induced by benzophenone photosensitization.

It is known that mixtures of oleic acid and sodium oleate spontaneously form vesicles in water. In this paper, we study this system in glycerol, and show that it also forms vesicles in this solvent, but with a considerably lower diameter. The critical vesicle concentration (cvc) was higher in glycerol (cvc = 27.1 mM) than in water (cvc = 0.10 mM). This finding was confirmed using an analogous system made of palmitoleic acid and palmitoleate. The vesicles in glycerol were characterized using small-angle neutron scattering (SANS) which showed that the fatty acids are embedded in a fluid bilayer phase. These fatty acid dispersions were used to produce emulsions in glycerol, using hexadecane as the oil component. We show that a higher energy is required to produce emulsions in glycerol than in water, probably because of the higher viscosity of glycerol. However, emulsions were shown to be stable in glycerol. Altogether, this shows that supramolecular self-assembly occurs in glycerol, and that emulsions can be successfully produced in this solvent.

Here in this communication, we report that combination of glycerol with scCO2 is a convenient tool for designing highly green catalytic processes. Indeed, as water, glycerol is cheap, abundant and non toxic. However, as compared to water, glycerol is poorly miscible and non reactive with scCO2 offering thus an alternative of choice for overcoming a lot of drawbacks encountered with water and scCO2 Key-words. Glycerol, scCO2, catalysis; green process, Heck coupling

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