Physicochemical Characterisation of Seeds, Oil and Defatted Cake of Three Hempseed Varieties Cultivated in Spain.

The increasing use of hempseed in food products highlights the need for a comprehensive database for scientific research and industrial applications. In food development, information about the techno-functional properties of raw materials plays a crucial role in determining the suitability of each product for specific applications. Thus, this study aims to characterise three hempseed varieties (Ferimon, Henola and Uso-31), comparing their physicochemical and nutritional compositions. Moreover, the study investigates the impact of hempseed varieties on the techno-functional, physical and thermal properties of the partially defatted hempseed flours (PDHFs) obtained from single screw pressing (SSP) oil extraction. The fatty acid and tocopherol profiles of the dehulled seeds and oil were also analysed. Significant variations in yield and physical properties were observed among hempseed varieties, influenced by genetics, adaptation to agro-climatic conditions and cultivation systems. Despite its lower yield (kg/ha), Uso-31 exhibited superior 1000-seed weight, dehulling yield and larger mean seed size (1.79 ± 0.02 mm). Hempseed oil was rich in unsaturated fatty acids, particularly linoleic (51.2-53.4 g/100 g oil) and α-linolenic (14.88-18.97 g/100 oil) acids, showing variations in γ- and α-tocopherols depending on the variety. The variety also influenced the least gelation concentration (LGC) and techno-functional properties such as water absorption capacity (WAC), emulsifying activity (EA) and emulsion stability (ES). SDS-PAGE and DSC measurements indicated the presence of 11S and 7S globulin proteins with denaturation temperatures above 87.8 °C. These findings confirm that the studied hempseed flours are valuable techno-functional and nutritional ingredients suitable for sustainable food formulations.

Novel Brazilian hop (Humulus lupulus L.) extracts through supercritical CO2 extraction: Enhancing hop processing for greater sustainability.

Hop cultivation has been increasing in the past decade in Brazil, demanding a better understanding of how the processing influences the national hop varieties. Despite the hop process being well-established in the producer countries, there is still room for optimization to reduce energy consumption for a more sustainable process. This study's main purpose was to understand the influence of drying and supercritical CO2 extraction on the quality of hop extracts. The hop quality during drying was evaluated regarding color, bitter acids, xanthohumol, total essential oil content, and volatile profile. Supercritical CO2 extraction yields, and bitter acid recovery were assessed by HPLC in a range of different temperatures (40 or 60 °C) and pressure (15, 20, 25, or 30 MPa) conditions. Hop processing was optimized to produce a greater extract quality from a Brazilian hop variety, saving energy and solvent consumption, and consequently, reducing the process footprint. Furthermore, this study established supercritical CO2 extraction conditions for Brazilian hop extract production, offering the national beer industry an alternative to overpriced products.

Microwave radiation induces modifications in the protein fractions of tef flours and modulates their derived techno-functional properties.

The impact of microwave (MW) treatments on the structure, solubility, and techno-functional properties of the proteins in starchy matrices is still poorly understood. This study aimed to investigate the effects of MW intensity by applying 1, 2, and 6 min of radiation on two tef flour varieties moistened at 15 % and 25 %. The fractionation method recovered ∼83 % of the total protein content in untreated flours. The interaction between treatment time and moisture content (MC) significantly influenced the extraction of protein fractions. Samples treated at 25 %MC showed significant reductions in albumins (up to -74 %), globulins (up to -79 %), and prolamins (up to -32 %). The SDS-extractable proteins of both tef flours presented similar molecular weights (12-100 kDa). SDS-PAGE analysis revealed decreased band intensity in MW-treated samples compared to untreated flours, and confocal analysis showed changes in the native state of proteins in treated samples. Shorter treatments at low MC significantly improved the emulsifying stability of tef flours, particularly in brown tef flour, with an enhancement of up to 203 %. The hydration properties significantly increased in flours treated at 25 %MC for 6 min. Pearson correlation analysis demonstrated the influence of treatment time and MC on protein recovery and functional properties of tef flours.

Lipase Inactivation Kinetics of Tef Flour with Microwave Radiation and Impact on the Rheological Properties of the Gels Made from Treated Flour.

In recent years, many efforts are being made to produce tef-based food for its nutritive and health-promoting advantages. Tef grain is always whole milled because of its tiny grain size and whole flours contain bran (pericarp, aleurone, and germ) where major non-starch lipids could be deposited along with the lipid-degrading enzymes: lipase and lipoxygenase. As lipoxygenase shows little activity in low moisture, the inactivation of lipase is the common objective for most heat treatments to extend the shelf life of flours. In this study, tef flour lipase inactivation kinetics via hydrothermal treatments assisted using microwaves (MW) were studied. The effects of tef flour moisture level (12%, 15%, 20%, and 25%) and MW treatment time (1, 2, 4, 6, and 8 min) on flour lipase activity (LA) and free fatty acid (FFA) content were evaluated. The effects of MW treatment on flour pasting characteristics and the rheological properties of gels prepared from the treated flours were also explored. The inactivation process followed a first-order kinetic response and the apparent rate constant of thermal inactivation increased exponentially with the moisture content of the flour (M) according to the equation 0.048·exp (0.073·M) (R2 = 0.97). The LA of the flours decreased up to 90% under the studied conditions. MW treatment also significantly reduced (up to 20%) the FFA level in the flours. The rheological study confirmed the presence of significant modifications induced by the treatment, as a lateral effect of the flour stabilization process.

Changes on Techno-Functional, Thermal, Rheological, and Microstructural Properties of Tef Flours Induced by Microwave Radiation-Development of New Improved Gluten-Free Ingredients.

Tef [Eragrostis tef (Zucc.) Trotter] flour is a gluten-free cereal rich in fiber, minerals, vitamins, and antioxidants, which offers a promising alternative for new food development. This study investigated the effect of microwave radiation (MW) on the techno-functional, thermal, rheological and microstructural properties of tef flours. White and brown tef grains were milled and microwaved at different moisture contents (MC) (15%, 20% and 25%) for a total irradiation time of 480 s. The morphological structure of tef flours was affected by MW treatment, and its particle size and hydration properties increased after the treatment. Lower peak, breakdown, and setback viscosities, up to 45%, 96%, and 67% below those of the control (untreated) samples, and higher pasting temperature, up to 8 °C in the 25% MC samples, were observed. From FTIR analysis a disruption of short-range molecular order was concluded, while DSC confirmed an increased stability of starch crystallites. Rheological analysis of the gels made from the treated samples revealed that MW had a structuring and stabilizing effect on all samples, leading to higher viscoelastic moduli, G' and G″, and the maximum stress the gels withstood before breaking their structure, τmax. The MC of the flours during the MWT drove the modification of the techno-functional properties of the tef flours and the gel rheological and thermal characteristics. These results suggest that MW-treated tef flours are potential ingredients for improving the technological, nutritional and sensory quality of food products.

Impact of Solubilized Substances on the Techno-Functional, Pasting and Rheological Properties of Ultrasound-Modified Rice, Tef, Corn and Quinoa Flours.

The modification of flours by ultrasound (US) treatments requires excess water to suspend the sample to be treated, which must be removed after treatment to recover the ultrasonicated flour. The aim of this study was to determine the influence that the water removal method has on the final characteristics of US-treated gluten-free flours (rice, brown tef, corn and quinoa). US treatment parameters were constant, and two water removal methods were studied: freeze-drying and centrifugation + drying. The elimination of water by centrifugation resulted in the loss of solubilized compounds from the treated flours, which led to important differences between the final characteristics of US-treated flours. Ultrasonication resulted in the reduction of flours' particle size and modification of their color parameters. Techno-functional properties were modified by US treatment, where the water removal method was more influential in whole grain samples (brown tef and quinoa). Few differences were found in thermal properties among pairs of US-treated samples, indicative that the effect caused to starch was mainly attributed to ultrasonication conditions than to the drying method. The water removal method markedly influenced the pasting properties of US-treated flours, resulting in lower profiles when freeze-drying was applied and higher profiles when flours were retrieved by centrifugation. Gels made with tef, corn and quinoa presented reduced tan(δ)1 values after sonication, while gels made with rice did not show any modification. The water removal method is a decisive step in US treatments, defining the final characteristics of the treated matter, and having a great influence in the modification attributed to ultrasonication.

Phenolic Compounds Recovery from Pomegranate (Punica granatum L.) By-Products of Pressurized Liquid Extraction.

This study aimed to valorize pomegranate by-products (peel and carpelar membranes-PPCM) through their high biological potential for phenolic compounds recovery. The influence of lower temperatures (40 and 60 °C) and pressures (20, 40, 60, 80, and 100 bar) than those generally used in pressurized liquid extraction (PLE) was evaluated through global extraction yield (X0), and qualitative and quantitative composition of the phenolic compounds. Chromatographic techniques were used to analyze the two treatments with the highest X0. Temperature, pressure, and their interaction had a significant influence on X0. The best phenolic compounds extraction conditions were using pressurized ethanol at 60 °C and 40 bar (extract 1-E1, 37% on d.b.) and 60 °C and 80 bar (extract 2-E2, 45% on d.b.). Nevertheless, E1 presented a significantly higher content of α, ß punicalagin, and ellagic acid (48 ± 2, 146 ± 11, and 25.6 ± 0.3 mg/100 g, respectively) than E2 (40 ± 2, 126 ± 4, and 22.7 ± 0.3 mg/100 g). Therefore, this study could validate the use of low pressures and temperatures in PLE to recover phenolic compounds from pomegranate residues, making this process more competitive and sustainable for the pomegranate industry.

Evaluation of antioxidant capacity, fatty acid profile, and bioactive compounds from buritirana (Mauritiella armata Mart.) oil: A little-explored native Brazilian fruit.

Buritirana (Mauritiella armata Mart.) is a fruit species native to the Amazon and Cerrado region, belonging to the Arecaceae family. It has high nutritional and functional potential, yet little explored. In this study, we evaluated for the first time the overall yield, behavior of total carotenoids in the extraction kinetics, fatty acid profile, bioactive compounds, and the antioxidant capacity of the oil from buritirana fractions obtained by supercritical CO2. The highest extraction yield was found in the pulp and whole without seed at 60 °C (18.06 ± 0.40 and 14.55 ± 1.10 g 100 g-1 of the freeze-dried sample (fdw), respectively), and in the peel at 40 °C (8.31 ± 0.73 g 100 g-1 fdw). During the extraction kinetics, the pulp had the highest yields of oil (41.57%) and total carotenoids (8.34 mg g-1) after 61 min at 40 °C. The antioxidant potential, fatty acid profile, and α-tocopherol content were dependent on both fraction and temperature, with oleic acid being the main fatty acid. The oil from the whole fraction without seed had the largest number (20) of identified phenolic compounds. The extraction at 60 °C reduced the relative intensity of most compounds in the whole without seed and pulp. Moreover, it increased the intensity of the compounds in the peel. These results suggest that buritirana is a good oil source with great bioactive potential to produce new products with functional claims.

Interactions of ß-carotene with WPI/Tween 80 mixture and oil phase: Effect on the behavior of O/W emulsions during in vitro digestion.

This study investigated the impact of adding ß-carotene on the structure of fresh O/W emulsions with different oil phase (sunflower oil-LCT or NEOBEE®1053-MCT) and emulsifiers (WPI, Tween 80 - T80 or WPI/T80 mixture). In this sense, the behavior of emulsions through the gastrointestinal tract, the stability and bioaccessibility of ß-carotene were also assessed. The ß-carotene reduced the interfacial tension of the LCT/MCT-water systems. The addition of ß-carotene promoted an increase of viscoelasticity of LCT/MCT-T80 (0.5%WPI/0.5%T80 and 1%T80 w/w) interfaces, but an increase of WPI content reduced the viscoelasticity of interfacial layers (LCT/MCT-1% WPI). These changes in the interface properties influenced the mean droplet size and ζ-potential of the fresh emulsions. LCT systems presented similar bioaccessibility/stability of ß-carotene. However, ß-carotene entrapped within protein-coated MCT droplets was more stable than within T80-MCT systems. Our results show that ß-carotene interacted with other ingredients of emulsions changing their properties and behavior under gastrointestinal tract as well as the stability/bioaccessibility of ß-carotene.

Extraction of bioactive compounds from defatted passion fruit bagasse (Passiflora edulis sp.) applying pressurized liquids assisted by ultrasound.

Passion fruit bagasse is a rich source of phenolic compounds, including piceatannol, a stilbene to which several biological activities are conferred. This work reports the application of pressurized liquid extraction (PLE) assisted by ultrasound (US) to intensify the extraction of phenolic compounds from defatted passion fruit bagasse (DPFB). PLE at different temperatures (65-75 °C) without and with different US powers (240-640 W) was performed to investigate the mechanism of the assisted process. The extracts were evaluated in terms of global, total phenolic (TP), piceatannol and total reducing sugar yields. The antioxidant capacity of the extracts was determined by FRAP and ORAC assays. PLE assisted by US increased the yields, resulting in 60% more TP and piceatannol. The observed yields suggest that the main mechanism driving PLE assisted by US from DPFB was the rise in temperature caused by the ultrasonic waves. Pearson coefficient revealed a strong correlation between antioxidant capacity and total phenolics and piceatannol yield. The three-line spline model was adequately fitted to the experimental curves, showing three extraction periods in which the recovery of TP and piceatannol was higher than 70% at the end of the falling extraction rate period. PLE assisted or not by US showed to be clean, efficient and green alternatives for the recovery of phenolic compounds. The findings of this work indicate that PLE assisted by US has a great potential to improve the extraction of bioactive compounds from natural products.

Impregnation of passion fruit bagasse extract in alginate aerogel microparticles.

Passion fruit bagasse extract (PFBE) is a rich source of polyphenols, including piceatannol. This work produced alginate (1, 2, 3 wt%) aerogel and investigated the impregnation of gallic acid (GA) and PFBE in alginate aerogel microparticles. The microparticles of ca. 100 µm in diameter were obtained by emulsion-gelation method, submitted to solvent exchange, wet impregnation (WI) and supercritical drying. Alginate aerogels derived from 1 wt% solution led to a higher GA loading and, therefore, this formulation was used to impregnate PFBE. The loading of PFBE, total phenolic, and piceatannol contents based on grams of raw aerogel were 0.62 g, 10.77 mg, and 741.85 µg, respectively, which means a loading efficiency of total phenolics and piceatannol of 47.1% and 34.7%. DSC analysis and X-ray diffraction showed that particles behave as amorphous materials and ORAC assay revealed that impregnated aerogel microparticles presented antioxidant capacity. Alginate aerogel microparticles presented as an appropriated material for drug loading, whereas WI and supercritical drying demonstrated to be useful techniques to load PBBE in aerogels.

Extraction of bioactive compounds from genipap (Genipa americana L.) by pressurized ethanol: Iridoids, phenolic content and antioxidant activity.

The search for compounds with functional properties from natural sources has grown in recent years as people have developed healthier habits. Therefore, the aim of this study was to evaluate the extraction of bioactive compounds from various parts of unripe genipap fruit (Genipa americana L.) by using pressurized ethanol to verify which part of the fruit provides the greatest recovery of the iridoids genipin and geniposide. Two process variables were studied: temperature (50 and 80°C) and pressure (2, 12 and 20 bar). The whole fruit and the peel, mesocarp, endocarp, endocarp+seeds and seeds of the fruit were studied. The endocarp presented with the highest recovery of genipin (48.6±0.6mg/g raw material) and the extraction from the mesocarp allowed a greater recovery of geniposide (59±1mg/g raw material). The highest values of total phenolic content were obtained with mesocarp extracts. The endocarp and mesocarp extracts presented the highest antioxidant activity as measured by FRAP and DPPH. These results are promising and support the use of unripe genipap fruit as a source of iridoids and natural antioxidants.