Sara Liparoti

Design and production of gentamicin/dextrans microparticles by supercritical assisted atomisation for the treatment of wound bacterial infections

In this work, the supercritical assisted atomisation (SAA) is proposed, for the first time, for the production of topical carrier microsystems based on alginate-pectin blend. Gentamicin sulphate (GS) was loaded as high soluble and hygroscopic antibiotic model with poor flowability. Particularly, different water solutions of GS/alginate/pectin were processed by SAA to produce spherical microparticles (GAP) of narrow size (about 2 μm). GS loading was varied between 20% and 33% (w/w) with an encapsulation efficiency reaching about 100%. The micronised powders also showed high flow properties, good stability and constant water content after 90 days in accelerated storage conditions. The release profiles of the encapsulated drug were monitored using vertical diffusion Franz cells to evaluate the application of GAP microsystems as self-consistent powder formulation or in specific fibres or gels for wound dressing. All formulations showed an initial burst effect in the first 6h of application (40-65% of GS loaded), and in particular GAP4 produced with a GS/alginate/pectin ratio of 1:3:1, exhibited the ability to release GS continuously over 6 days. Antimicrobial tests against Staphylococcus aureus indicated that GS antibiotic activity was preserved at 6 days and higher than pure GS at 12 and 24 days for all SAA formulations, especially for GAP1.

Fast mold surface temperature evolution: relevance of asymmetric surface heating for morphology of iPP molded samples

It is widely accepted that mold temperature has a strong effect on the amount of molecular orientation and morphology developed in a non-isothermal flowing melt. In this work, this effect was investigated in fast and asymmetric thermal conditions. Therefore, a well-characterized isotactic polypropylene was injected in a rectangular mold cavity conditioned by a purpose developed thin electric heater. Temperature evolution on the mold surface influences the cooling rates near the surface that, in turn, reduces flow stresses and facilitates molecular relaxation. Moreover, asymmetrical thermal conditions have a strong influence on the melt flow field by changing its distribution along the cavity thickness. As a consequence, the morphology distribution of the molded samples was asymmetric and showed complex and peculiar features. It was accurately characterized by optical microscopy and FESEM analysis and compared with the orientation distribution obtained by birefringence measurements.

Supercritical Assisted Atomization: Polyvinylpyrrolidone as Carrier for Drugs with Poor Solubility in Water

Supercritical assisted atomization (SAA) is an efficient technique to produce microparticles and composite microspheres formed by polymers and pharmaceutical compounds. In this work polyvinylpyrrolidone (PVP) was proposed as carrier for pharmaceutical compounds that show a poor solubility in water medium. Indeed, this polymer is hydrosoluble and can be generally used to enhance the dissolution rate of hydrophobic compounds when finely dispersed in it. However, it is difficult to obtain coprecipitates with a uniform dispersion of the active molecule using other micronization techniques. The experiments were performed using ethanol as solvent; SAA plant was operated at 40°C and 76 bar in the saturator and 70°C and 1.6 bar in the precipitator. Three different dexamethasone/polymer weight ratios were selected: 1/2, 1/4, and 1/8. Produced composite particles showed a regular, spherical shape and a mean diameter ranging from about 0.8 to 1 μm, depending on the polymer/drug weight ratio. Dissolution analysis demonstrated that microparticles containing a lower drug amount show a higher dissolution rate.

Fast cavity surface temperature evolution in injection molding: control of cooling stage and final morphology analysis

Fast mold surface temperature evolution in injection molding improves the surface finishing and replicability of the molded parts, and may significantly reduce frozen-in orientation. In this paper the effect of a fast control of cavity surface temperature evolution on the morphology and processing conditions of iPP molded parts has been characterized. Phenomena not previously encountered, such as a double pressure packing step when the cavity surface heating lasts longer than the packing step, have been pointed out. Significant effects on the samples frozen-in orientation have been observed by optical microscopy and confirmed by X-ray analysis. AFM analysis shows that it is possible to achieve isotropic morphology with cavity surface temperature kept constant at 150 °C for a long heating time and low holding pressure.

Fast temperature evolution on the mold surface: Analysis and simulation

Injection molding is one of the most widespread processes in the polymeric manufacturing field, because it allows to have a good reproducibility of the molded objects in a very short cycle time. The possibility to control mold temperature during the process, so as to have high temperature during filling and low temperature during cooling, is considered very attractive for several reasons.To this purpose, fast mold surface heating is proposed in this paper. A mold temperature rise of about 100°C in 1-2 seconds was obtained by a thin electric heater layered on the mold surface. A fast cooling phase and, as a consequence, a fast cycle time is not lost because the heating layer thickness is small.Injection molding tests were performed with a very accurately characterized iPP as far as rheology, quiescent crystallization, effect of flow on nucleation and spherulitic growth rates and spherulitic/fibrillar transition.A series of tests with different heating powers (steady mold wall temperatures) held constant fr...

Rapid control of mold temperature during injection molding process

The control of mold surface temperature is an important factor that determines surface morphology and its dimension in thickness direction. It can also affect the frozen molecular orientation and the mold surface replicability in injection molded products. In this work, thin thermally active films were used to quickly control the mold surface temperature. In particular, an active high electrical conductivity carbon black loaded polyimide composites sandwiched between two insulating thin polymeric layers was used to condition the mold surface. By controlling the heating time, it was possible to control precisely the temporal variation of the mold temperature surface during the entire cycle. The surface heating rate was about 40°C/s and upon contact with the polymer the surface temperature decreased back to 40°C within about 5 s; the overall cycle time increased only slightly. The effect on cross section sample morphology of samples of iPP were analyzed and discussed on the basis of the recorded temperature evolution.

Micromechanical Characterization of Complex Polypropylene Morphologies by HarmoniX AFM

This paper examines the capability of the HarmoniX Atomic Force Microscopy (AFM) technique to draw accurate and reliable micromechanical characterization of complex polymer morphologies generally found in conventional thermoplastic polymers. To that purpose, injection molded polypropylene samples, containing representative morphologies, have been characterized by HarmoniX AFM. Mapping and distributions of mechanical properties of the samples surface are determined and analyzed. Effects of sample preparation and test conditions are also analyzed. Finally, the AFM determination of surface elastic moduli has been compared with that obtained by indentation tests, finding good agreement among the results.

Effect of fast mold surface temperature evolution on iPP part morphology gradients

The control of mold surface temperature is an important factor that affects the sample surface morphology as well as the structural gradients (orientation crystal size, and type) as well as cooling stresses. The frozen layer thickness formed during the filling stage also has a very significant effect on the flow resistance and thus on the resulting pressure drop and flow length in thin wall parts. The possibility to have a hot mold during filling and a quick cooling soon afterward is a significant process enhancement particularly for specialized applications such as micro injection molding and for the reproduction of micro structured surfaces. Up to now, several methods (electromagnetic, infrared, hot vapor fleshing etc,) were tried to achieve fast temperature evolution of the mold. Unfortunately, all these methods require a complex balance between thermal and mechanical problems, equipment cost, energy consumption, safety, molding cycle time and part quality achievable.In this work, a thin electrical res...

Rapid control of mold temperature during injection molding process: Effect of packing pressure

A thorough analysis of the effect of operative conditions of injection molding process on the morphology distribution inside the obtained molded is performed, with particular reference to semi- crystalline polymers. In particular, fully characterized injection molding tests are presented using an isotactic polypropylene, previously carefully characterized as far as most of properties of interest. The effects of mold temperature and packing conditions are analyzed. The mold temperature was controlled by a thin heating device, composed by polyimide as insulating layer and polyimide loaded carbon black as electrical conductive layer, that is able to increase temperature on mold surface in few seconds (70°C/s) by joule effect and cool down soon after. The shear layer thickness in the molded is reduced in the samples produced at high mold temperatures, that means high electrical power and long heating time, and this reduction is more significant at lower packing pressures, indeed, at 360bar as packing pressure...

Hydrophobicity Tuning by the Fast Evolution of Mold Temperature during Injection Molding

The surface topography of a molded part strongly affects its functional properties, such as hydrophobicity, cleaning capabilities, adhesion, biological defense and frictional resistance. In this paper, the possibility to tune and increase the hydrophobicity of a molded polymeric part was explored. An isotactic polypropylene was injection molded with fast cavity surface temperature evolutions, obtained adopting a specifically designed heating system layered below the cavity surface. The surface topology was characterized by atomic force microscopy (AFM) and, concerning of hydrophobicity, by measuring the water static contact angle. Results show that the hydrophobicity increases with both the temperature level and the time the cavity surface temperature was kept high. In particular, the contact angle of the molded sample was found to increase from 90°, with conventional molding conditions, up to 113° with 160 °C of cavity surface temperature kept for 18 s. This increase was found to be due to the presence of sub-micro and nano-structures characterized by high values of spatial frequencies which could be more accurately replicated by adopting high heating temperatures and times. The surface topography and the hydrophobicity resulted therefore tunable by selecting appropriate injection molding conditions.