The effect of the degradation process on the physicomechanical properties of the PCL/HA composites

Kompozyty na bazie polikaprolaktonu z dodatkiem wypełniacza w postaci włókien hydroksyapatytowych są jednym z potencjalnych materiałów do zastosowań inżynierii tkankowej. Materiały te odznaczają się nie tylko odpowiednią porowatością i wytrzymałością mechaniczną, lecz także bioaktywnością, biokompatybilnością i bioresorbowalnością. Z punktu widzenia możliwości aplikacyjnych danego materiału niezwykle istotna jest kontrola procesu degradacji kompozytu w czasie, tak aby rusztowanie mogło zapewnić stabilność mechaniczną do momentu odbudowy ubytku. W pracy przedstawiono wyniki badań dotyczące wpływu procesu degradacji na właściwości fizykomechaniczne opracowanych porowatych kompozytów na bazie polikaprolaktonu (PCL) z dodatkiem zsyntezowanych włókien hydroksyapatytu (HA) o zróżnicowanej morfologii. Szczególną uwagę zwrócono na wpływ zsyntezowanego proszku na zmianę właściwości fizykomechanicznych kompozytów w procesie degradacji. Próbki do badań otrzymano metodą liofilizacji. Proces degradacji badano poprzez pomiar ubytku masy, zmiany mikrostruktury, powierzchni właściwej, gęstości i wytrzymałości na ściskanie w czasie. Pomiary prowadzono po 3, 6 i 12 tygodniach inkubacji w soli fizjologicznej buforowanej fosforanem (PBS). Wyniki badań wykazały, że proces degradacji badanych kompozytów jest bardzo wolny, a dodatek zsyntezowanego HA nieznacznie go przyspiesza. Ubytek masy kompozytu po 12 tygodniach inkubacji w PBS wynosił zaledwie 0,47%. Procesowi degradacji towarzyszy spadek gęstości i wzrost powierzchni właściwej materiału w czasie. Porównanie wytrzymałości opracowanych kompozytów PCL/HA przed i po 12 tygodniach inkubacji w PBS, pozwala wnioskować, że dodatek zsyntezowanego hydroksyapatytu wpływa na wzrost wytrzymałości kompozytów w czasie (nawet do 20%).Polycaprolactone-based composites with filler in the form of hydroxyapatite fibers are one of the potential materials for tissue engineering applications. These materials are characterized not only by adequate porosity and mechanical strength, but also by bioactivity, biocompatibility and bioresorbability. From the point of view of the applicability of a given material, it is extremely important to control the degradation process of the composite over time, so that the scaffold can provide mechanical stability until the defect is restored. The paper presents the results of the study of the effect of the degradation process on the physicomechanical properties of the developed porous composites based on polycaprolactone (PCL) with the addition of synthesized hydroxyapatite (HA) fibers of different morphologies. In the study, special attention was paid to the effect of the synthesized powder on the change of physicomechanical properties of the composites during the degradation process. Samples for the study were obtained by freeze-drying method. The degradation process was studied by measuring weight loss, changes in microstructure, specific surface area, density and compressive strength over time. Measurements were conducted after 3, 6 and 12 weeks of incubation in PBS (phosphate-buffered saline). The results showed that the addition of synthesized HA slightly accelerates the degradation process of PCL/HA composites. Nevertheless, the degradation process is very slow. The weight loss of the composite after 12 weeks of incubation in PBS was only 0.47%. The degradation process is accompanied by a decrease in density and an increase in the specific surface area of the material over time. A comparison of the strength of the developed PCL/HA composites before and after 12 weeks of incubation in PBS, allows us to conclude that the addition of synthesized hydroxyapatite affects the increase in the strength of the composites over time (up to 20%)

Effects of Sterilization and Hydrolytic Degradation on the Structure, Morphology and Compressive Strength of Polylactide-Hydroxyapatite Composites

Composites based on polylactide (PLA) and hydroxyapatite (HA) were prepared using a thermally induced phase separation method. In the experimental design, the PLA with low weight-average molar mass (Mw) and high Mw were tested with the inclusion of HA synthesized as whiskers or hexagonal rods. In addition, the structure of HA whiskers was doped with Zn, whereas hexagonal rods were mixed with Sr salt. The composites were sterilized and then incubated in phosphate-buffered saline for 12 weeks at 37 °C, followed by characterization of pore size distribution, molecular properties, density and mechanical strength. Results showed a substantial reduction of PLA Mw for both polymers due to the preparation of composites, their sterilization and incubation. The distribution of pore size effectively increased after the degradation process, whereas the sterilization, furthermore, had an impact on pore size distribution depending on HA added. The inclusion of HA reduced to some extent the degradation of PLA quantitatively in the weight loss in vitro compared to the control without HA. All produced materials showed no cytotoxicity when validated against L929 mouse skin fibroblasts and hFOB 1.19 human osteoblasts. The lack of cytotoxicity was accompanied by the immunocompatibility with human monocytic cells that were able to detect pyrogenic contaminants

Calcination and ion substitution improve physicochemical and biological properties of nanohydroxyapatite for bone tissue engineering applications

Abstract Nanohydroxyapatite (nanoHAP) is widely used in bone regeneration, but there is a need to enhance its properties to provide stimuli for cell commitment and osteoconduction. This study examines the effect of calcination at 1200 °C on the physicochemical and biological properties of nanoHAP doped with magnesium (Mg2+), strontium (Sr2+), and zinc (Zn2+). A synergistic effect of dual modification on nanoHAP biological properties was investigated. The materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), BET analysis, Fourier-transform spectroscopy, and thermal analysis methods. Furthermore, ion release tests and in vitro biological characterization, including cytocompatibility, reactive oxygen species production, osteoconductive potential and cell proliferation, were performed. The XRD results indicate that the ion substitution of nanoHAP has no effect on the apatite structure, and after calcination, β-tricalcium phosphate (β-TCP) is formed as an additional phase. SEM analysis showed that calcination induces the agglomeration of particles and changes in surface morphology. A decrease in the specific surface area and in the ion release rate was observed. Combining calcination and nanoHAP ion modification is beneficial for cell proliferation and osteoblast response and provide additional stimuli for cell commitment in bone regeneration