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STAGE I - 2022

O1. Anthocyanins separation and purification for new smart biopackaging based on xanthan

The plant material required for the study was represented by blueberries, currants and two varieties of blackberries (noted blackberries SV and blackberries BT) (Figure 1) harvested in 2021 at full maturity from the Rădăuţi area, Suceava county and Brăeşti area, Botoşani county. The plant material was kept in the freezer (-18 °C) until the moment of extraction.

Figure 1. The plant material used in this study to obtain the extracts

For extraction, the samples were thawed and crushed (Figure 2A,B). The extracts were prepared by mixing plant product with acidified methanolic solution under stirring at room temperature, vacuum filtration and centrifugation (Figure 2C). The characteristic supernatant of each plant material was collected and concentrated in a rotary evaporator (Figure 2D). The obtained extracts were lyophilized for 48 h (Figure 2E) and dried to constant mass in the vacuum desiccator.

Figure 2. (A) Crushing black currants for extraction; (B) Remaining residues after extraction; (C) Primary solutions ; (D) Concentrated extracts; (E) Appearance of extracts after lyophilization; (F) Extracts in 40% ethanol.

O2. Synthesis of the xanthan matrix in order to be facile used for food packaging

Figure 3. Materials used to obtain new XG-based biomaterials: Glycerol diglycidyl ether (R1); 1,4-Butanediol diglycidyl ether (R2); Epichlorohydrin (R3).

Figure 4. Optical microscopy images showing the appearance of XG-based cryogels.

STAGE II - 2023

The activities accomplished according to the proposed objectives within AntoSensECOPACK project indicated the following:

Xanthan-based cryogels were successfully prepared by freeze-thawing technique, stabilization being achieved both by means of physical interactions between polymer chains and by the use of a cross-linking agent, namely, 1,4-butanediol diglycidyl ether.
The incorporation of polyphenolic blueberry extracts in different concentrations within xanthan-based biopolymeric matrices was successfully achieved with the aim to increase their stability, and to obtain biomaterials with new features.
The obtained materials were characterized structurally, morphologically, but also from mechanical and rheological point of view; their stability in various environmental conditions, antioxidant and antimicrobial activities were also evidenced.
The obtained results indicated that the porous cryogels containing blueberry extracts exhibited swelling, wetting, mechanical and rheological properties in accordance with (i) the amount of the extract entrapped, (ii) the method used for extract loading, and (iii) the nature of crosslinking, i.e. physical or chemical.
The stability of blueberry extract was significantly increased by encapsulation within xanthan-based matrices compared to the native extract. Blueberry extract also maintained its antioxidant activity through inclusion, and also conferred to cryogel matrices a significant antimicrobial activity against Salmonella typhimurium, Escherichia coli and Listeria monocytogenes.

STAGE III - 2024

The activities accomplished according to the proposed objectives within AntoSensECOPACK project indicated the following:

The color stability of anthocyanin-loaded xanthan-based materials was monitored under normal exposure conditions where the temperature and brightness of the storage room were characteristic of the day and night cycle. The evolution of the colorimetric parameters Δa*, Δb* and ΔC* for cryogels as films was followed during 50 days.
Over 50 days of storage, the investigated materials remain stable and do not result in structural changes characteristic of the red flavinium ion or the green quinoid form, and the pH sensor quality of the samples is not altered.
The thermal behavior of the obtained films was studied using thermogravimetric analysis; the anthocyanin-loaded xanthan-based materials presented four stages of degradation, which suggests an increased thermal stability for these networks.
Dissemination of the results: 5 published papers, 1 published book chapter, 1 submitted paper, 1 submitted patent and 13 participations in national/international conferences (4 oral communications and 9 posters).