A cada dia é mais crescente a necessidade e interesse no desenvolvimento de embalagens competitivas e com maior valor agregado. Visando atender a necessidade de consumidores cada vez mais exigentes e preocupados com o meio ambiente, este trabalho propôs o uso do pigmento natural antocianina no desenvolvimento de filmes biodegradáveis para potencial uso como embalagem inteligente, indicadora de mudança de pH. Os filmes foram elaborados pela técnica de casting tendo como formulação base fécula de mandioca (Manihot esculenta Crantz), argila esmectita sódica, glicerol, etanol e água, e incorporados com duas concentrações de antocianina (0,05 e 0,10) g/100 g de solução filmogênica, e em uma segunda fase, ácido cítrico foi incorporado à matriz polimérica a fim de estudar a influência do pH da solução filmogênica (2,8 e 4,3) sobre o desempenho do filme empregado como embalagem. Os filmes foram avaliados quanto as suas propriedades mecânicas (resistência máxima à tração e porcentagem de elongação na ruptura), físico-químicas (atividade de água, umidade, espessura), de barreira (permeabilidade ao vapor dágua e ao oxigênio) e análise de mudança de cor. Em seguida à caracterização, a atividade indicadora de pH foi testada com peixe cru embalado em recipientes de vidro tampados com o filme. Os recipientes foram acondicionados em temperatura ambiente e sob três temperaturas distintas de refrigeração, sendo que recipientes vazios também fechados com o filme foram usados como controle. A avaliação da atividade indicadora de pH foi realizada por meio da análise de mudança de cor do filme correlacionada com o pH do peixe. Os resultados obtidos foram promissores, uma vez que os filmes avaliados se mostraram bons indicadores de pH, ao mudarem de cor à olho nu em resposta à variação do pH, sendo essa mudança mais acentuada em filmes com maior conteúdo de antocianina. / The interest and need for the development of more competitive, higher value-added packages grow faster each day. For attending the needs of a more demanding, environmentally-concerned group of consumers, the present work proposes the use of natural anthocyanin pigment for the development of biodegradable films to be used as intelligent packaging material capable of indicating pH change. These films, made by employing a technique known as casting, consist of a basic formulation of cassava starch (Manihot esculenta Crantz), sodium smectite clay, glycerol, ethanol, and water, combined with two concentrations of anthocyanin (0.05 and 0.10) g/100 g of a filmogenic solution. In a second phase, citric acid was added to the polymer matrix in order to study the influence of the filmogenic solution pH (2.8 and 4.3) on the packaging performance of the films. These materials were assessed according to their mechanical properties (tensile strength at break and elongation at break percentage), physical and chemical properties (water activity, moisture content and thickness), barrier properties (water vapor and oxygen permeability), and color change. After this characterization, the pH-indicating activity was tested with raw fish stored in glass containers sealed with the film. Such containers were firstly exposed to room temperature and subsequently to three different refrigeration temperatures. Similarly, some empty containers also sealed with the same film were used as control. The assessment of the pH-indicating activity was undertaken by analyzing the color change of the film correlated with the pH of the fish. Promising outcomes seemed to have been achieved, since the films that were assessed proved to be efficient pH indicators. The color change was visible to the naked eye in response to pH variation, and such a change was particularly strong in the films with higher anthocyanin content.

Mainly used food packaging materials are petro-chemical based polymers which present environmental problems since they are not biodegradable and ecologically sustainable. In this study, biodegradable biofilms are produced from xylan, extracted from cotton stalk which is an agricultural biowaste without nutritional value. Antimicrobial property was given to the biofilms with either titanium dioxide sol-gel coatings or titanium dioxide powder addition into the biofilm forming solutions. The antimicrobial activities of biofilms were tested against Escherichia coli. Among two different sol-gels coated and at different temperatures dried biofilms, BWX and CSX-50 biofilms treated at 120&deg / C and coated with SiO2/TiO2 showed 88&plusmn / 1% and 75&plusmn / 2% antimicrobial activities, respectively. Same samples treated at the same conditions but coated with non-SiO2 added TiO2 sol-gel yielded 63&plusmn / 3% and 63&plusmn / 2% antimicrobial activities, respectively after 2 h black light illumination. So, it was determined that the highest photocatalytic antimicrobial property was achieved with SiO2/TiO2 coated biofilms. Moreover different concentrations of TiO2 powder were integrated into xylan based biofilms and 100% photocatalytic inactivation was gathered at 5% (w/w) TiO2 addition achieved at both biofilms at the end of 90 min black light illumination. Biodegradability properties of the biofilms were investigated in soil burial test during 180 days and 10% (w/w) TiO2 powder added CSX-50 biofilms were recorded to be 91% biodegradable where non-powder added blank biofilms was found to be 95% biodegradable.

Xylan was extracted from cotton waste, characterized by DSC and TGA analysis and used in biodegradable film production. Pure cotton waste xylan did not form film. The presence of an unknown compound, as an impurity, yielded composite films. The unknown compound was determined as a phenolic compound, and most probably lignin, by using DSC and TGA analysis and Folin-Ciocalteau method. The effects of xylan concentration of the film forming solutions, glycerol (plasticizer) and gluten additions on thickness, mechanical properties, solubility, water vapor transfer rate, color and microstructure of the films were investigated. Films were formed within the concentration range of 8-14%. Below 8%, film forming solutions did not produce films, whereas xylan concentrations above 14% was not used because of high viscosity problems. The average tensile strength, strain at break, water vapor transfer rate and water solubility of the cotton waste xylan films were determined as about 1.3 MPa, 10%, 250 g/m2.24h and 99%, respectively. The addition of glycerol as the plasticizer resulted in a decrease in the tensile strength and an increase in strain at break. The change in water solubility due to the addition of glycerol was very small. In addition, water vapor transfer rate and the deviation of the color from the reference color for the plasticized films were found to be higher than the unplasticized films. The effect of addition of wheat gluten in cotton waste xylan film forming solutions on film formation was investigated at different concentration ratios. However, the incorporation of wheat gluten worsen the film quality.

A cada dia é mais crescente a necessidade e interesse no desenvolvimento de embalagens competitivas e com maior valor agregado. Visando atender a necessidade de consumidores cada vez mais exigentes e preocupados com o meio ambiente, este trabalho propôs o uso do pigmento natural antocianina no desenvolvimento de filmes biodegradáveis para potencial uso como embalagem inteligente, indicadora de mudança de pH. Os filmes foram elaborados pela técnica de casting tendo como formulação base fécula de mandioca (Manihot esculenta Crantz), argila esmectita sódica, glicerol, etanol e água, e incorporados com duas concentrações de antocianina (0,05 e 0,10) g/100 g de solução filmogênica, e em uma segunda fase, ácido cítrico foi incorporado à matriz polimérica a fim de estudar a influência do pH da solução filmogênica (2,8 e 4,3) sobre o desempenho do filme empregado como embalagem. Os filmes foram avaliados quanto as suas propriedades mecânicas (resistência máxima à tração e porcentagem de elongação na ruptura), físico-químicas (atividade de água, umidade, espessura), de barreira (permeabilidade ao vapor dágua e ao oxigênio) e análise de mudança de cor. Em seguida à caracterização, a atividade indicadora de pH foi testada com peixe cru embalado em recipientes de vidro tampados com o filme. Os recipientes foram acondicionados em temperatura ambiente e sob três temperaturas distintas de refrigeração, sendo que recipientes vazios também fechados com o filme foram usados como controle. A avaliação da atividade indicadora de pH foi realizada por meio da análise de mudança de cor do filme correlacionada com o pH do peixe. Os resultados obtidos foram promissores, uma vez que os filmes avaliados se mostraram bons indicadores de pH, ao mudarem de cor à olho nu em resposta à variação do pH, sendo essa mudança mais acentuada em filmes com maior conteúdo de antocianina. / The interest and need for the development of more competitive, higher value-added packages grow faster each day. For attending the needs of a more demanding, environmentally-concerned group of consumers, the present work proposes the use of natural anthocyanin pigment for the development of biodegradable films to be used as intelligent packaging material capable of indicating pH change. These films, made by employing a technique known as casting, consist of a basic formulation of cassava starch (Manihot esculenta Crantz), sodium smectite clay, glycerol, ethanol, and water, combined with two concentrations of anthocyanin (0.05 and 0.10) g/100 g of a filmogenic solution. In a second phase, citric acid was added to the polymer matrix in order to study the influence of the filmogenic solution pH (2.8 and 4.3) on the packaging performance of the films. These materials were assessed according to their mechanical properties (tensile strength at break and elongation at break percentage), physical and chemical properties (water activity, moisture content and thickness), barrier properties (water vapor and oxygen permeability), and color change. After this characterization, the pH-indicating activity was tested with raw fish stored in glass containers sealed with the film. Such containers were firstly exposed to room temperature and subsequently to three different refrigeration temperatures. Similarly, some empty containers also sealed with the same film were used as control. The assessment of the pH-indicating activity was undertaken by analyzing the color change of the film correlated with the pH of the fish. Promising outcomes seemed to have been achieved, since the films that were assessed proved to be efficient pH indicators. The color change was visible to the naked eye in response to pH variation, and such a change was particularly strong in the films with higher anthocyanin content.

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With the growing concern of the accumulation of plastic-based food packaging waste, the search for bio-based biodegradable packages is on the rise. These materials differ from their petro-based counterparts in their degradation rates, which are much higher in the former. Not only do bio-based biodegradable materials degrade faster during post-usage processes but also they age faster during usage and storage, which affects their performance and functionality. The application of noninvasive testing methods with the capability to report on the matrix’s state could assist in the development of a more ubiquitous way to assess ageing in food packaging, particularly in biodegradable ones. To this end, the performance of a luminescence spectroscopy technique based on three luminescent probes, one intrinsic to the matrix and two added, was monitored and the sensitivity of the probes to report on ageing was analyzed. Biodegradable films were made of 2% gelatin (type A) and 0.5% glycerol (plasticizer). Gelatin contains an intrinsic fluorophore, the aromatic amino acid tyrosine (Tyr), which can report on the molecular mobility of a matrix. Additionally, the films were doped with two extrinsic fluorophores, Fast Green FCF (FG) at 0.124 mM and pyranine (Pyr) at 0.05 mM, which can report on the physical state and available free water within a matrix, respectively. Films were casted onto plastic Petri dishes and stored at five relative humidities (RHs), namely 2.5, 25, 33, 53, and 75%, for five weeks with measurement collection every week. Films were tested using fluorescence spectroscopy at excitation and emission range wavelengths optimized depending on the assessed probe. Additional measurements to determine moisture content, changes in secondary protein structure using FTIR spectroscopy, and mechanical properties using a Universal Testing Machine in tensile mode aided in the evaluation of the sensitivity of the luminescent probes in sensing ageing. Luminescent probes, intrinsic or added, have the capability to assess the physical state of the films in situ and can provide molecular level sensing of their local environment. Tyr emission showed a sharp increase in fluorescence intensity in films stored at low RH as a function of time. FG showed a similar pattern to that of Tyr but higher sensitivity to changes along the observed period. The two characteristics emission bands of Pyr provide information on the state of water within the matrix. Although the results on this probe hinted microstructural rearrangements within the films as a function of time, the sensitivity of this probe was not high enough at the conditions evaluated and provided limited information on films’ solvation. The sensitivity of the luminescent probes to changes during ageing were revealed through correlation of the photophysical properties of the two effective probes, Tyr and FG, and the mechanical properties of the films at different RH through storage. Both methods, mechanical and optical, were similarly sensitive to changes during ageing particularly after 3-week storage. However,, it can be speculated that because of the different scales at which optical and mechanical measurements report (local vs. bulk), the methods, they could also complement each other. These findings suggest that, in principle, a luminescence spectroscopy technique using intrinsic and extrinsic probes can replace mechanical testing to noninvasively monitor structural changes and stability of biodegradable packaging as a function of time.