Tableting properties of microcrystalline cellulose obtained from wheat straw measured with a single punch bench top tablet press.

The objective of this work was to study the relation between the manufacturing conditions of microcrystalline cellulose (MCC), its physicochemical properties and its tableting behavior. Two different preparation procedures were used to produce MCC from wheat straw, utilizing an acid hydrolysis method, either using only sulfuric acid or combination of sulfuric and hydrochloric acid. The tableting behavior of obtained MCC samples and mixtures of MCC with ibuprofen was studied using a dynamic powder compaction analyzer. It was observed that some of the obtained MCC samples showed better flowing properties than commercially available Vivapur® PH101 and also very high values of tensile strength, solid fraction and elastic recovery. This can be linked with its good compaction behavior, but on the other hand it can cause problems with the disintegration of the tablets. In mixtures with ibuprofen, MCC samples showed lower values of tensile strength, while on the other hand elastic recovery did not seem to be much affected, still exhibiting very high values. According to the obtained results, it can be concluded that MCC obtained from the agricultural waste could have satisfactory properties for tablet preparation by the direct compression method. Further studies are needed to optimize process conditions in order to achieve better physicochemical characteristics, especially in terms of elastic recovery.

Supercritical CO2 - assisted production of PLA and PLGA foams for controlled thymol release.

Amorphous, medical grade poly(d,l-lactic acid) (PLA) and poly(d,l-lactic-co-glycolic acid) (PLGA) were used to develop systems for controlled release of a natural bioactive substance - thymol. Supercritical carbon dioxide (scCO2) was successfully used both as an impregnation medium for thymol incorporation into the polymer matrix and a foaming agent in a single-step batch process. Impregnation of samples using low to moderate scCO2 densities (273 kg/m3 and 630 kg/m3) and short processing times (2 h and 4 h) enabled thymol loading of 0.92%-6.62% and formation of microcellular foams upon system depressurization. Thymol effect on structural and thermal properties on foamed samples was proven by FTIR and DSC. The effect of CO2 under elevated pressure on the neat polymers was analysed by high pressure DSC. Foaming of polymers with lower molecular weight by CO2 of higher density yielded foams with smaller pores. All tested foams released thymol in a controlled manner in phosphate buffered saline (PBS) at 37 °C within 3 to 6 weeks. Higher loading and lower cell density favoured thymol release rate, while its concentration in PBS for the tested period depended on foam interaction with the medium. Representative PLGA foam sample with the highest thymol loading (6.62%) showed controlled thymol release within 72 h in mediums having pH values from 1.1 to 7.4.

Supercritical CO2 impregnation of PLA/PCL films with natural substances for bacterial growth control in food packaging.

Biodegradable polymers with antibacterial properties are highly desirable materials for active food packaging applications. Thymol, a dietary monoterpene phenol with a strong antibacterial activity is abundant in plants belonging to the genus Thymus. This study presents two approaches for supercritical CO2 impregnation of poly(lactic acid)(PLA)/poly(ε-caprolactone)(PCL) blended films to induce antibacterial properties of the material: (i) a batch impregnation process for loading pure thymol, and (ii) an integrated supercritical extraction-impregnation process for isolation of thyme extract and its incorporation into the films, operated in both batch or semi-continuous modes with supercritical solution circulation. The PCL content in films, impregnation time and CO2 flow regime were varied to maximize loading of the films with thymol or thyme extract with preserving films' structure and thermal stability. Representative film samples impregnated with thymol and thyme extract were tested against Gram (-) (Escherichia coli) and Gram(+) (Bacillus subtilis) model strains, by measuring their metabolic activity and re-cultivation after exposure to the films. The film containing thymol (35.8 wt%) showed a strong antibacterial activity leading to a total reduction of bacterial cell viability. Proposed processes enable fast, controlled and organic solvent-free fabrication of the PLA/PCL films containing natural antibacterial substances at moderately low temperature, with a compact structure and a good thermal stability, for potential use as active food packaging materials.

Novel modified nanocellulose applicable as reinforcement in high-performance nanocomposites.

The influence of modification and vacuum/supercritical CO2 (scCO2) drying methods on the surface properties, morphology and thermal stability of cellulose nanocrystals (NC) was presented in this study. Introduction of reactive vinyl groups on NC surface was performed by either direct esterification with oleic acid, linseed or sunflower oil fatty acids; or by amidation of maleic acid/ethylene diamine with methyl ester of fatty acid. Obtained modified NC (m-NC) were characterized using FTIR and Raman spectroscopy; and by determination of acid, iodine and ester values. Structural analysis of m-NC showed varieties of forms, from spongy to nanostructural non-uniform layered morphology with observable agglomeration, which confirmed morphology dependence on modification/processing methods Thermogravimetry-MS spectrometry showed different thermal stability and degradation pathways of NC/m-NC. Incorporation of 1 wt% of reactive m-NC in unsaturated polyester lead to high performance nanocomposites and contributed to increase of stress at break in the range from 76 to 93%.

Application of cellulose acetate for controlled release of thymol.

Cellulose acetate (CA) was investigated as a carrier towards development of material with controlled release of thymol as a natural substance with strong antibacterial properties using high pressure techniques. Effect of thymol content on CA was confirmed by SEM, FTIR and DSC methods. Kinetic of thymol release from CA was tested using simulated gastric and intestinal fluids (hydrochloric acid and phosphate buffer saline). Results were correlated with Korsmeyer-Peppas and Weibull model. Depending on the thymol content and chemical nature of the release medium, the time of thymol release varied from one to three days indicating CA as a promising carrier of thymol with potential uses from medicine to agriculture. The impregnated CA showed antibacterial activity against 23 tested bacterial strains including methicillin-resistant Staphylococcus aureus (MRSA) which is particularly important bearing in mind that this strain causes fatal infections in humans and animals.