Iván Jesús Jiménez-Pulido

This study aimed to develop a nutraceutical gummy candy enriched with hydrolysed hemp (Cannabis sativa L.) as a natural antioxidant and antihypertensive ingredient. Three European cultivars—Futura 75, Henola, and KC Zuzana—were cultivated under rainfed (RF) and irrigated (RFCI) conditions and assessed for nutritional composition and bioactivity. Henola variety showed the most favourable profile, showing the highest protein content under RFCI (29.4 g 100 g⁻¹ d.m.) and the greatest phenolic concentration under RF (15.8 µmol GAE g⁻¹ d.m.), with 35–40% higher antioxidant capacity than the other cultivars. Henola (RF) was selected for enzymatic hydrolysis with Ultraflo^® XL, which enhanced total phenolics and antioxidant capacity by 65% and 58%, respectively, stabilizing after 18 h. Incorporation of the hydrolysate (0.66%) into a pectin-based gummy significantly (p < 0.05) increased total phenolic content by 52% and antioxidant capacity by up to 60% compared with controls. After simulated digestion, bioactivity decreased by 30–45% but remained higher than controls. The incorporation of 0. 66 g of hydrolysed ingredient in 100 g of gummy increased ACE inhibition by 10% after digestion, probably associated with the peptides released during the digestion, confirming hydrolysed hemp as a stable multifunctional ingredient for plant-based nutraceutical formulations targeting oxidative stress and hypertension.

The food industry generates substantial waste, contributing to environmental challenges, such as pollution and greenhouse gas emissions. Utilizing by-products, particularly fruit peels that are rich in fiber, antioxidants, and vitamins, presents a sustainable approach to reducing waste, while enhancing the nutritional value of food products. Specifically, peach peel can be used to produce gluten-free flours, with increased fiber content and antioxidant properties. Extrusion technology is a highly effective method for developing these functional flours, as it improves digestibility, reduces anti-nutrients, and enhances nutrient bioavailability. This study investigates the potential of combining corn flour with peach peel flour, derived from Royal Summer peachs (RSF), at different concentrations (0%, 5%, and 15%). A factorial experimental design was utilized to evaluate the impact of RSF incorporation on the proximate composition, antioxidant capacity, and functional properties of the flour. The results indicate that flours containing 15% RSF demonstrated significant improvements in terms of the dietary fiber content (5.90 g per 100 g⁻¹) and antioxidant capacity (ABTS^•+ 745.33 µmol TE per 100 g⁻¹), meeting the “source of fiber” labelling requirements. The glycemic index of the 15% RSF flour was reduced to 78.09 compared to non-enriched flours. The functional properties of the flour, such as swelling and gelation capacities, were also enhanced with RSF incorporation. These findings highlight the potential of RSF-enriched flours in regard to the development of sustainable, health-promoting, plant-based, and gluten-free flours.

Efficient development of effective functional foods and nutraceuticals requires adequate estimation methods of the bioaccessibility of their bioactive compounds. Specially grain-based nutraceuticals and functional ingredients are often enriched in bound/low bioavailable bioactive phytochemicals. The objective of this work was to evaluate the differences in applying static or dynamic digestion models for the estimation of bioaccessibility of antioxidants present in cereal grain-based/fiber-rich ingredients produced using enzymatic hydrolysis and sprouting processes. Main liberated phenolic compounds, antioxidant activity (ABTS^•+ and ORAC) and ferric reducing capacity were evaluated in the samples following three digestion protocols with differences based on their dynamism: static, semi-dynamic and dynamic. The samples digested with the dynamic method showed higher antioxidant and reducing capacities than those digested with the static and semi-dynamic protocols. The results obtained from the digests with the dynamic model showed a total phenol content (TPs) ranging from 1068.22 to 1456.65 μmol GAE 100 g⁻¹ and antioxidant capacity values from 7944.62 to 15,641.90 μmol TE 100 g⁻¹ (ORAC) and from 8454.08 to 11,002.64 μmol TE 100 g⁻¹ (ABTS^•+), with a reducing power ranging from 2103.32 to 2679.78 mmol Fe reduced 100 g⁻¹ (FRAP). The dynamic character of the protocols used for developing bioactive cereal-based foods significantly affects the estimation of their bioaccessibility, probably giving a better approach to their potential bioavailability in in vivo systems.

Nutraceuticals obtained from sprouted wheat and oat grains and processing by-products (bran and hull, respectively) naturally containing antioxidant and anti-inflammatory compounds were evaluated. The objective of this study was the development of a cereal-based nutraceutical formula combining extracts from sprouts and by-products and the exploration for potential synergetic effects in their bioactive properties. The antioxidant and anti-inflammatory capacities, glycemic index, phytic acid, and β-glucan of individual wheat bran hydrolysate (EH-WB), sprouted wheat (SW), oat hull hydrolysate (EH-OH), sprouted oat (SO), and combined ingredients (CI 1, CI 2, and CI3) were used to tailor an optimal nutraceutical formula. The three blend ingredients (CI 1, CI2, and CI3) were formulated at different ratios (EH-WB:SW:EH-OH:SO; 1:1:1:1, 2:1:2:1, and 1:2:1:2, w:w:w:w, respectively). The resulting mixtures showed total phenol (TPs) content ranging from 412.93 to 2556.66 µmol GAE 100 g⁻¹ and antioxidant capacity values from 808.14 to 22,152.54 µmol TE 100 g⁻¹ (ORAC) and 1914.05 to 7261.32 µmol TE 100 g⁻¹ (ABTS^•+), with Fe³⁺ reducing ability from 734. 02 to 8674.51 mmol reduced Fe 100 g⁻¹ (FRAP) for the individual ingredients produced from EH-WB and EH-OH, where high antioxidant activity was observed. However, the anti-inflammatory results exhibited an interesting behavior, with a potentially synergistic effect of the individual ingredients. This effect was observed in CI2 and CI3, resulting in a higher ability to inhibit IL-6 and TNF-α than expected based on the anti-inflammatory values of their individual ingredients. Similar to the antioxidant properties, oat-based ingredients significantly contributed more to the anti-inflammatory properties of the overall mixture. This contribution is likely associated with the β-glucans and avenanthramides present in oats. To ensure the bioaccessibility of these ingredients, further studies including simulated digestion protocols would be necessary. The ingredient formulated with a 2:1 hydrolysate-to-sprout ratio was the most effective combination, reaching higher biological characteristics.

Wheat bran (WB) and oat hull (OH) are two interesting undervalued cereal processing sources rich in total dietary fibre (TDF) and other associated bioactive compounds, such as β-glucans and polyphenols. The aim of this study was to optimise a combination chemical (enzymes) and physical (high hydrostatic pressure-temperature) strategies to increase the bioaccessibility of bioactive compounds naturally bound to the bran and hull outer layers. WB and OH were hydrolysed using food-grade enzymes (UltraFloXL and Viscoferm, for WB and OH, respectively) in combination with HPP at different temperatures (40, 50, 60 and 70 °C) and hydrolysis either before or after HPP. Proximal composition, phytic acid, β-glucans, total phenolics (TPs) and total antioxidant activity (TAC) were evaluated to select the processing conditions for optimal nutritional and bioactive properties of the final ingredients. The application of the hydrolysis step after the HPP treatment resulted in lower phytic acid levels in both matrices (WB and OH). On the other hand, the release of β-glucan was more effective at the highest temperature (70 °C) used during pressurisation. After the treatment, the TP content ranged from 756.47 to 1395.27 µmol GAE 100 g⁻¹ in WB, and OH showed values from 566.91 to 930.45 µmol GAE 100 g⁻¹. An interaction effect between the temperature and hydrolysis timing (applied before or after HPP) was observed in the case of OH. Hydrolysis applied before HPP was more efficient in releasing OH TPs at lower HPP temperatures (40–50 °C); meanwhile, at higher HPP temperatures (60–70 °C), hydrolysis yielded higher TP values when applied after HPP. This effect was not observed in WB, where the hydrolysis was more effective before HPP. The TP results were significantly correlated with the TAC values. The results showed that the application of optimal process conditions (hydrolysis before HPP at 60 or 70 °C for WB; hydrolysis after HPP at 70 °C for OH) can increase the biological value of the final ingredients obtained.

Previous studies demonstrated that enzymatic hydrolysis enhances wheat bran (WB) biological properties. This study evaluated the immunostimulatory effect of a WB hydrolysate (HYD) and a mousse enriched with HYD (MH) before and after in vitro digestion on murine and human macrophages. The antiproliferative activity of the harvested macrophage supernatant on colorectal cancer (CRC) cells was also analyzed. MH showed significantly higher content than control mousse (M) in soluble poly- and oligosaccharides (OLSC), as well as total soluble phenolic compounds (TSPC). Although in vitro gastrointestinal digestion slightly reduced the TSPC bioaccessibility of MH, ferulic acid (FA) levels remained stable. HYD showed the highest antioxidant activity followed by MH, which demonstrated a greater antioxidant activity before and after digestion as compared with M. RAW264.7 and THP-1 cells released the highest amounts of pro-inflammatory cytokines after being treated with 0.5 mg/mL of digested WB samples. Treatment with digested HYD-stimulated RAW264.7 supernatant for 96 h showed the most anticancer effect, and spent medium reduced cancer cell colonies more than direct WB sample treatments. Although a lack of inner mitochondrial membrane potential alteration was found, increased Bax:Bcl-2 ratio and caspase-3 expression suggested activation of the mitochondrial apoptotic pathway when CRC cells were treated with macrophage supernatants. Intracellular reactive oxygen species (ROS) were positively correlated with the cell viability in CRC cells exposed to RAW264.7 supernatants (r = 0.78, p < 0.05) but was not correlated in CRC cells treated with THP-1 conditioned media. Supernatant from WB-stimulated THP-1 cells may be able to stimulate ROS production in HT-29 cells, leading to a decrease of viable cells in a time-dependent manner. Therefore, our present study revealed a novel anti-tumour mechanism of HYD through the stimulation of cytokine production in macrophages and the indirect inhibition of cell proliferation, colony formation, and activation of pro-apoptotic proteins expression in CRC cells.

Gluten-free products (GFP) currently are the fastest-growing category of baked goods probably due to the high worldwide incidence of celiac disease (CD). Refined rice is one of the most used cereal flour for GFP development, due to its high content in starch and good technological aptitude. However, its low content in fibre, protein and minerals has awakened a recent interest as alternative to balance the GF flour formulas. Teff is a cereal with high levels in fibre and antioxidants compounds but the lack of gluten results in very limited techno-functional properties. Extrusion is a thermal technology that allows to combine flours, overcoming negative impacts on quality characteristics. This study evaluated the effect of twin-screw extruder on rice-teff (white and brown) mixtures with different teff concentrations (25, 50 and 75%) on their antioxidant, glycaemic index and techno-functional properties. The results showed than the high shear–temperature process produced important modifications on the flour, which were confirmed using scanning electron microscopy (SEM). Significant increases in total dietary fibre (16 to 100% increase) were observed in teff containing flours, due to carbohydrate–lipid–protein complexes, which lead to resistant starch, with no significant increase in rice flour. Hydration and pasting properties were significantly (p > 0.05) affected by extrusion, and the effect was related to the concentration of teff used. The thermal process showed a decrease in total phenol (TP) content for rice; however, extrusion enhanced the release of total phenol in rice-teff blends, which was reflected on the antioxidant activities of blend flours, especially those prepared with brown teff.

Oat consumption has increased during the last decade because of the health benefits associated with its soluble dietary fiber (β-glucan), functional proteins, lipids, and the presence of specific phytochemicals, such as avenanthramides. Oat is consumed mainly as whole grain, and the hull (seed coat), comprising 25–35% of the entire grain, is removed, generating a large amount of waste/by-product from the milling industry. The objective of this study was to evaluate the use of biotechnological strategies, such as sprouting for oat grain (OG) and hydrolysis for oat hull (OH), to enhance antioxidant and anti-inflammatory properties and lower the glycemic index (GI). Sprouting produced significant (p ≤ 0.05) increases in free (32.10 to 76.62 mg GAE (100 g)⁻¹) and bound phenols (60.45 to 124.36 mg GAE (100 g)⁻¹), increasing significantly (p ≤ 0.05) the avenanthramide (2c, 2p and 2f) soluble phenolic alkaloid content and anti-inflammatory properties of OG. On the other hand, the hydrolysis of OH using Viscoferm (EH2-OH) and Ultraflo XL (EH21-OH) increased by 4.5 and 5-fold the release of bound phenols, respectively; meanwhile, the use of Viscoferm increased the 4.55-fold soluble β-glucan content in OH, reaching values close to those of OG (4.04 vs. 4.46 g (100 g)⁻¹). The study shows the potential of both strategies to enhance the nutritional and bioactive properties of OG and OH and describes these processes as feasible for the industry to obtain an ingredient with high antioxidant and anti-inflammatory activities. Single or combined biotechnological tools can be used on oat grains and hulls to provide nutraceutical ingredients.