Assessing texturometer-derived rheological data for predicting the printability of gummy formulations in SSE 3D printing.

Semi-solid extrusion (SSE), an additive manufacturing technique, is gaining significant attention for the printing of thermosensitive drugs. Hydrogels, one of the materials used in SSE, have emerged as a focus in pharmaceutical applications due to their ability to control the release of therapeutic agents spatially and temporally. Understanding the non-Newtonian flow and evaluating the mechanical properties of hydrogel-based materials during extrusion is, however, essential for successful 3D printing. Thus, users often find themselves conducting both rheological and texture profile analyses to characterize the hydrogel. While texturometers are primarily used to evaluate mechanical or sensory properties, viscosity measurements are typically performed using rotational rheometers or viscometers. In this study, we demonstrated how comparable rheological information can be obtained using a texturometer as a capillary rheometer. By preparing similar formulations to a previous study, we compared the rheological data obtained from a rotational rheometer to the data obtained from the texturometer. The means of the parameters obtained by fitting the data from both techniques to the power law model showed insignificant differences. In addition, three clusters were formed based on the flow behaviour and printability of the samples using principal component analysis. Furthermore, the printability was predicted using the samples' consistency and flow indexes, and the regression coefficient was 96.62 and 60.03% for capillary and rotational flow parameters, respectively. This approach thus holds the potential to streamline the time, expertise and equipment required for the rheological characterization of hydrogels for applications in semi-solid extrusion.

Evaluation of the printability of agar and hydroxypropyl methylcellulose gels as gummy formulations: Insights from rheological properties.

The trial-and-error method currently used to create formulations with excellent printability demands considerable time and resources, primarily due to the increasing number of variables involved. Rheology serves as a relatively rapid and highly beneficial method for assessing materials and evaluating their effectiveness as 3D constructs. However, the data obtained can be overwhelming, especially for users lacking experience in this field. This study examined the rheological properties of formulations of agar, hydroxypropyl methylcellulose, and the model drug caffeine, alongside exploring their printability as gummy formulations. The gels' rheological properties were characterized using oscillatory and rotational experiments. The correlation between these gels' rheological properties and their printability was established, and three clusters were formed based on the rheological properties and printability of the samples using principal component analysis. Furthermore, the printability was predicted using the sample's rheological property that correlated most with printability, the phase angle δ, and the regression models resulted in an accuracy of over 80%. Although these relationships merit confirmation in later studies, this study suggests a quantitative definition of the relationship between printability and one rheological property and can be used for the development of formulations destined for extrusion 3D printing.

Polymer Supercritical CO2 Foaming under Peculiar Conditions: Laser and Ultrasound Implementation.

The two-step batch foaming process of solid-state assisted by supercritical CO2 is a versatile technique for the foaming of polymers. In this work, it was assisted by an out-of-autoclave technology: either using lasers or ultrasound (US). Laser-aided foaming was only tested in the preliminary experiments; most of the work involved US. Foaming was carried out on bulk thick samples (PMMA). The effect of ultrasound on the cellular morphology was a function of the foaming temperature. Thanks to US, cell size was slightly decreased, cell density was increased, and interestingly, thermal conductivity was shown to decrease. The effect on the porosity was more remarkable at high temperatures. Both techniques provided micro porosity. This first investigation of these two potential methods for the assistance of supercritical CO2 batch foaming opens the door to new investigations. The different properties of the ultrasound method and its effects will be studied in an upcoming publication.

Crystallization of α-glycine by anti-solvent assisted by ultrasound.

Crystallization of α-glycine by addition of an anti-solvent (ethanol) assisted by ultrasound is studied. The experiments of crystallization are conducted at 303.15 K in a solution of 150 ml with continuous agitation by a magnetic rod. Ultrasound is then applied at powers ranging from 8 to 41 W thanks to an ultrasonic horn at 20 kHz. The supersaturation ratio (S) is followed throughout all the experiment. At the end of the experiment, the suspension is filtered, the solid is washed with ethanol and dried at 333.15 K. The resulting crystals are characterized by their final size distributions measured by laser granulometry, their morphologies observed by scanning electronic microscope (SEM) and their crystalline structures by differential scanning calorimetry (DSC). The influence of ultrasonic power (continuous 13, 28 and 40 W or pulsed modes), measured by calorimetry method, is studied for different addition rates (0.05 to 0.36 g of ethanol/min). Ultrasound permits to reduce the metastable zone width and to decrease the size of crystals due to an increase of the nucleation rate. The rate of de-supersaturation is higher in presence of ultrasound, inducing a higher nucleation rate, a higher growth rate or both. At 40 W, the decrease of supersaturation is faster, and the crystallization is finished in 40 min instead of 80 min (at 13 and 28 W) or 120 min without ultrasound. The use of pulsed ultrasound (50 on/50 off) is interesting from an economic point of view because similar results are obtained: comparable size distributions and resembling concentration profiles.