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- Molecular mobility, composition and structure analysis in glycerol plasticised chitosan filmsPublication . Fundo, Joana; Fernandes, Rui; Almeida, Pedro M.; Carvalho, Alexandra; Feio, Gabriel; Silva, Cristina L. M.; Quintas, MafaldaThis study was developed with the purpose to investigate the effect of polysaccharide/plasticiser concentration on the microstructure and molecular dynamics of polymeric film systems, using transmission electron microscope imaging (TEM) and nuclear magnetic resonance (NMR) techniques. Experiments were carried out in chitosan/glycerol films prepared with solutions of different composition. The films obtained after drying and equilibration were characterised in terms of composition, thickness and water activity. Results show that glycerol quantities used in film forming solutions were responsible for films composition; while polymer/total plasticiser ratio in the solution determined the thickness (and thus structure) of the films. These results were confirmed by TEM. NMR allowed understanding the films molecular rearrangement. Two different behaviours for the two components analysed, water and glycerol were observed: the first is predominantly moving free in the matrix, while glycerol is mainly bounded to the chitosan chain.
- Relationship between molecular mobility, microstructure and functional properties in chitosan/glycerol filmsPublication . Fundo, Joana; Carvalho, Alexandra; Feio, Gabriel; Silva, Cristina L. M.; Quintas, Mafalda A.C.Foods are partially crystalline partially amorphous systems. Edible films are considered good models for food systems due to their interesting physical properties, quite straightforward matrices, and easy reproduction. Chitosan is a semicrystalline biopolymer, biocompatible, biodegradable, with antimicrobial activity and filmogenic properties, thoroughly used in edible films' studies. This work aims to investigate the relationship between chitosan films' molecular relaxation time, their microstructure (crystallinity) and functional properties. Analyses were carried out using data on chitosan/glycerol films prepared with different polymer/plasticisant concentrations. Results demonstrate that there is a relationship between macroscopic properties and water and glycerol relaxation times. Moreover, results show that while water is free in the matrix, glycerol is linked to the chitosan polymeric chains, decreasing intermolecular attractions and increasing free volume, thus facilitating molecular migration. Also the data analysis reveals the usefulness of NMR and molecular mobility studies in the matrix for characterisation and development of polymeric structures. Industrial relevance: NMR spectroscopy is currently one of the key methods for food characterisation. Foodstuff is a complex matrix including many different compounds with different chemical structures, concentrations, solubility, properties and nutritional values. From a fundamental perspective, foods are mainly edible and digestible biopolymers that are partially crystalline/partially amorphous and thus edible films, specifically chitosan/glycerol films can be very interesting food model systems for mobility and microstructure studies. Studies on water and solids' mobility and thermo-mechanical properties in food systems (real or model systems),are fundamental to fully attain food physical properties and stability. These studies may be extremely useful for food product and process design, safety and sensorial attributes and also for better understanding and predicting, for example, food storage stability conditions.
- Fresh-cut melon quality during storage: an NMR study of water transverse relaxation timePublication . Fundo, Joana F.; Amaro, Ana L.; Madureira, Ana Raquel; Carvalho, Alexandra; Feio, Gabriel; Silva, Cristina L. M.; Quintas, MafaldaMolecular mobility is a fundamental parameter which reflects the dynamic properties of food components and contributes to food degradation reactions comprehension. Fresh-cut fruits have become an important food market segment. However, processing of fruits promotes faster its physiological deterioration, biochemical changes and microbial degradation. The purpose of this work was to use NMR methodology as a tool to evaluate fresh-cut fruit quality, during storage at refrigerated conditions. The fresh-cut melon transverse relaxation time (T2) was measured for a period of 7 days of storage at 5 °C. The relationship between the obtained values, microstructure and quality parameters was investigated. In general, results show the existence of one class of water fluidity in the system, the one present in cells after processing. T2, a measure of this fluidity, is affected by the processing and storage time. Also, it is possible to find a close relationships between T2 and quality parameters of total colour difference (TCD), firmness and aw. As T2 increases TCD also increases, while firmness and aw decrease. These results highlight the usefulness of NMR methodology application in food science.