New well characterized process and formulated pilot-products (in Collaboration with Companies) [GRIP - D2.6.2]

NODES – Nord Ovest Digitale e Sostenibile FLAGSHIP PROJECT GRIP SPOKE 2 –GREEN TECHNOLOGIES AND SUSTAINABLE INDUSTRIES DELIVERABLE D2.6.2 “New well characterized process and formulated pilot-products (in Collaboration with Companies) ” REPORTING PERIOD Period covered: from M8 to M 32 Periodic report date and version: 30-09-2025 Deliverable # Responsible Arlorio RM2 Responsible Arlorio This report is part of the project NODES which has received funding from the MUR – M4C2 1.5 of PNRR funded by the European Union - NextGenerationEU (Grant agreement no. ECS00000036) 1 Glossary Definition Hub Coordinator (HC) The Hub Coordinator represents the single point of contact for the implementation of the innovation ecosystem towards the MUR. It carries out the management and coordination activities of the innovation ecosystem, receives the fundings, verifies, and transmits to the MUR the reporting of the activities carried out by the Spoke and their affiliates. National Recovery and Resilience Plan (NRRP) This document uses the Italian acronym for the NRRP, which is PNRR (Piano Nazionale della Ripresa e Resilienza) Research Program Manager The person who will be the responsible for the overall scientific contents of the NODES project. The NODES will appoint the Research Program Manager. It refers to “Responsabile del Programma di Ricerca” in the MUR’s Call of proposal for “Ecosistemi di Innovazione” NODES’ Research and innovation program NODES’ Research and Innovation program is articulated in specific programs for each Spoke, with the aim to promote and support applied research on topics consistent with the Intelligent Specialization Strategy, with the guidelines of the 2021-2027 partnership agreement scheme, with regional operational plans and regional and national research and innovation priorities. Although NODES’ Spokes are concentrated on different themes, they will organize their activities and actions within a common framework – NODES’ Booster Methodoloy Spoke Coordinator The University in charge of coordinating the Spoke’s ecosystem. It refers to “Spoke” in the MUR’s Call of proposal for “Ecosistemi di Innovazione” Spoke Data Manager The person who will be the responsible for the monitoring and management of data generated at the Spoke level. The Spoke Coordinator will appoint the Spoke Data Manager. Spoke Partner The entity associated to the Spoke Coordinator. It can be an Innovation Cluster, Competence Center, Research Center related to the Spoke’s ecosystem and contributes to achieve objectives and impact under the Spoke’ leadership and management. It refers to “soggetti affiliati” in the MUR’s Call of proposal for “Ecosistemi di Innovazione”. Spoke Project manager The person who will be the responsible for the management, coordination and progress of the project at the Spoke level. The Spoke Coordinator will appoint the Spoke Project Manager. Spoke research and innovation program NODES’ Research and Innovation program is articulated in specific programs for each Spokes. The spoke will leverage a consolidated collaboration with leading private and public companies and will focus the applied research activity on technological domains and applications that can favour the integration of SMEs into new value chains. Spoke Scientific and Technical Manager The person who will be the responsible for the overall scientific contents of the project at the Spoke level. The Spoke Coordinator will appoint the Spoke Scientific and Technical Manager. Spoke Stakeholders Committee (SC) Consultation structure formed by relevant stakeholders (Government, universities, companies, civil society, third sector, etc.) Spoke Thematic General target focus and domain of the Spoke research. Spoke Topics Specific areas/lines of development within the Spoke. Spoke Work Package Leader At the Spoke level, Work Packages (WPs) will be organized by WP leaders, who will be responsible for performance evaluation and reporting. Flagship Project Main research project at the Spoke level with the goal of prototyping, testing, demonstrating the research activities towards higher TRLs. 2 List of Deliverables D. No Name Lead Benefi ciary Type Dissemi nation Level Due Date New Due Date (if delay) Delivery Date (actual) [number] [name] [short name] [R — Document, report] [DEM — Demonstrat or, pilot, prototype] [DEC — Websites, patent filings, videos, etc] [DATA — data sets, microdata, etc] [DMP — Data Manageme nt Plan] [ETHICS] [SECURITY] [OTHER] [PU — Public] [SEN — Sensitive ] [R] [C] [S] [month number] [dd/mm/ yyyy] [dd/mm/yyy y] D2.1 Data about chemical and nutritional profiling of raw wastes and by products UPO R PU M14 (Febbrai o 2024) D2.2.1 On line lab-scale technical multi-device for waste processing* UPO Other (material) PU M18 (June) D2.2.2 Delivery of protocols (lab-scale) ready to scale-up the production of new high-value material (in collaboration with Companies) UPO R PU M22 D2.3.1 New data about valorized matrices characterization and high value products UPO R PU M28 D2.3.2 New characterized ingredients/mat erials for food, nutraceuticals, pharma and UPO Other (material) PU M30 3 cosmetic applications D2.4.1 New data about sustainable production of new materials from biomasses UPO R PU M24 D2.4.2 New characterized materials from biomasses UPO Other (material) (& Report) PU M30 D2.5.2 Porous sorbents from biomasses valorization UPO Other (material) (& Report) PU M30 D2.6.1 New material produced at pilot scale ready to the formulation or co-formulation (in collaboration with Companies) UPO Other (material) (& Report) PU M32 30-09.2025 D2.6.2 New well characterized process and formulated pilot-products (in collaboration with Companies) UPO R/Other (Material) PU M32 30-09-2025 D2.7 Report on the adsorption and/or catalytic performances of porous solids derived from biomasses valorization and non-recyclable plastic wastes UPO R PU M32 4 A) INTRODUCTION The main outcome reported in this Deliverable is related to the description of the design and the production of three pilot scale model products (food supplements; cosmetics) formulated using selected valorised (and characterized ingredients) as described in D.2.3.1, D.2.3.2, D. 2.4.2 and listed in D 6.2.2. After the complete characterization of the best performing (single or combined) bio-based and green technological processes, the work allowed to obtain some well characterized ingredient, ready to be scaled up as well as to be used in model products. B) ROLE OF PARTNERS As described in the preliminary Deliverables as well as detailed in the Project (RM2, GRIP PROJECT), all the Partners worked in synergy (and also complementarily) in order i) to estimate the value of each single bio-based/green process, ii) to evaluate the best performing approaches useful to valorise/upcycle raw organic materials (liquid and solid; biomasses from environmental origin; waste and by-products from agrifood chains. The main outcome of the overall work were: - new processed valorised raw material - new ingredients/fractions from processed raw materials, ready to be used in different areas (chemical, nutraceutical , cosmetical, pharmaceutical) - new “model products” as proof of concepts for the entire RM2 research activities, formulated and developed in collaboration with some Companies. Moreover, each Partner developed specific solution that – beside the three final model products here described – will be probably able in the future enabling new applied researches or new processes, allowing to obtain more products and more applications in a real industrial environment (e.g. the valorization of recalcitrant biomasses useful to be added as “additives” in cement or in plastic materials, or porous material for environmental applications, as described in D2.5.2 and D2.7). Unit DSF-UPO, depending on i) the broad availability of valorised materials (essentially 5 derived from the cocoa bean husks, apple pomace and fruit pomace up-cycling), produced in small pilot scale, and ii) depending on the large collaboration with pharmaceutical, nutraceutical and cosmetic Companies, proceeded with the production of two food supplements and a cosmetic formula (emulgel), as following described. The Companies involved in this part of the Project were Procemsa Company (Turin; the Company funded a PhD program); ProgeFarm Company (Novara) and APTsol Company (Novara). The collaboration with the companies was strategic especially in the phases of the product formulation and pilot production. C) EXPLANATION OF THE WORK CARRIED OUT AND OVERVIEW OF THE PROGRESS The three proof of concepts (POCs) here considered the final model products as result of the overall research, were prepared using: ▪ Prebiotic fiber/antioxidant polyphenols from cocoa bean husks ▪ Fiber from apple pomace ▪ Phloretin/phlorizin/polyphenol rich ingredients from apple pomace ▪ Polyphenols rich extract from blueberry pomace 6 Model product 1 – Capsules (food supplement) – developed in collaboration with Farmaceutici Procemsa Company Rationale: the main idea related to the development of a new food supplement, was focused on the valorization of cocoa fibers from cocoa bean shells processed as described in Deliverables (more particularly selecting the process developed by ultrasounds and enzyme-driven hydrolysis of carbohydrates, in order to obtain a prebiotic-like oligosaccharides-rich up-cycled dietary fiber. The bioactivity of this ingredient was established in collaboration with other NODES project (particularly GREENVAL UPO POC project and some Industrial POCs), confirming the usefulness in boosting the production in vitro of Short Chain Fatty Acids (SCFAs). These overall activities can be considered a success correlated with the intra-fertilization system of research of Nodes. This ingredient was formulated together with the ingredient obtained from the valorized apple pomace extract, enriched in phloridzin and polyphenols. The rationale was to develop a food supplements useful to control the glycemic index (apple ingredient) also regulating the microbiota (cocoa ingredient rich in prebiotic fibers). In synthesis, in collaboration with Farmaceutici Procemsa S.p.A., capsules of 0.5 mL were produced containing 0.3 g of cocoa bean shells-derived ingredients (obtained with ultrasound and enzymatic hydrolysis, as described in previous deliverables). This specific treatment resulted in the highest content of oligosaccharides, fermentable sugars, and antioxidant activity among the tested preparations. The formulation also included 3% (w/w) of dried apple pomace extract, a source particularly rich in phloridzin, which was incorporated to enhance the nutraceutical profile of the product. The capsules were successfully produced using standard encapsulation processes and demonstrated good technological and chemical stability upon preliminary evaluation (Figure 2). Moreover, a pilot production were obtained in collaboration with the Company, active also in the formulation step. Initial tests also indicated that the capsules possessed satisfactory gastric resistance, suggesting that the release of bioactive compounds may primarily occur in the intestinal environment—an aspect favorable for the delivery of prebiotic oligosaccharides and antioxidant polyphenols. The combination of cocoa shell and apple pomace extracts therefore represents a promising formulation for supporting gut health and counteracting oxidative stress, as well as potentially modulating glycaemia. The achieved results will permit more investigation (in vitro and in vivo trials are planned with future projects). 7 Figure 1. Spray-drying system Figure 2. Tablets obtained using a capsule-filling machine based on cocoa and apple pomace extract. 8 Model product 2 – Tablets (food supplement) – Developed in collaboration with Proge Farm Srl and APTSol Srl Companies Rationale: the main idea was to valorize the antioxidant and anti-inflammatory property of the polyphenol-rich extract prepared from cocoa bean shells, as described in the previous Deliverables. The tablets (beside the large use of the capsules) are still considered a pharmaceutical form useful to deliver bioactive compounds, as well as largely used both in pharma and food areas. More precisely, in collaboration with Progefarm Srl, tablets were first formulated and then produced using a base mixture composed of lactose, crospovidone, and povidone, to which micronized cocoa bean shells-derived ingredients were added at two different inclusion levels (5 and 10% w/w) (Figure 4). The mixture ensured suitable flowability and compressibility, allowing for efficient tableting without the need for additional excipients. The formulations containing 10% cocoa shell powder were successfully compressed, yielding tablets with uniform weight and appearance, appropriate hardness, and good disintegration properties. However, preliminary scaling-up simulations indicated the need to further evaluate the behavior of the ingredients under larger industrial production conditions. Indeed, when increasing the cocoa shell content to 15%, difficulties arose during compression due to poor powder flow and the irregular shape of the resulting tablets. These findings suggest that 10% represents a practical upper limit for cocoa shell incorporation under the current formulation and processing conditions, and further optimization will be required to improve processability at higher inclusion levels. The produced tablets showed good physical stability over time and retained a significant antioxidant capacity/anti-inflammatory capacity attributable to the polyphenolic fraction of cocoa shells. These properties make the tablets suitable candidates for further nutraceutical developments, particularly in formulations targeting oxidative stress reduction and general metabolic well-being, also permitting to add more additional ingredients (e.g. specific vitamins). 9