The use of silk proteins sericin (SS) and fibroin (SF) has been increased for biomedical applications. In order to improve their behavior inside of biological environment, silk biomaterials must be treated after their manufacturing by means of diverse methods. These include ethanol post-treatments to increase their crystallinity, mechanical properties and water stability. In this study, the effect of ethanol post-treatments on the properties of silk protein materials was evaluated. Defective cocoons and silk fibrous waste (SW) were used to obtain silk sericin sponges (S-SS) and silk fibroin films (F-SF), respectively. Two ethanol treatments were evaluated in SS and SF: immersion (I) and solvent vapor annealing (SVA). Morphological modifications induced by ethanol post-treatments were studied by scanning electron microscopy (SEM). Conformational structure of the samples was analyzed by attenuated total reflectance-Fourier-transform infrared spectroscopy (ATR-FTIR), and the thermal properties were evaluated by differential scanning calorimetry (DSC) measurements. SEM images revealed that ethanol process induces changes in treated F-SF and S-SS, the material surfaces are more roughness, and these effects were more pronounced in samples treated by I than that subjected to SVA. As a result of the ethanol treatments, the ATR-FTIR and DSC results showed an increment in relative content of β-sheet structures in both silk protein materials. The results suggest that ethanol post-treatments induce conformational transitions and morphological modifications in S-SS and F-SF that should be considered to select the post-treatment conditions according to the biomedical application requirements.
Silk fibroin (SF) is a protein polymer claimed to have outstanding potential for medical applications. However, because of the manufacturing process, materials from regenerated SF exhibit a higher percentage of amorphous structures. The amorphous structures cause the material to be water soluble and can significantly limit its applications in wet biological environments. In order to increase the amount of crystalline structures and decrease the water solubility of SF materials, post-treatment with alcohols is usually employed. SF can be obtained from silk fibrous wastes (SFW), usually discarded in silk textile processes. This represents an opportunity to produce materials with high added value from low-cost natural sources. In this study, SF was obtained from SFW, and films were made thereof followed by a post-treatment by immersion or in a saturated atmosphere of methanol (MeOH) or ethanol (EtOH), using different exposure times. The resulting films were analyzed according to crystallinity, the percentage of crystalline and amorphous structures, and thermal stability. Also, water absorption and weight loss in aqueous media were determined. The results showed a significant increase in crystalline structures in all treated samples, varying according to the type and time of exposure to post-treatment conducted. The highest increase was shown in the case of the post-treatment by immersion in MeOH for 1 h, with a 23% increase over the untreated sample. This increase in crystallinity was reflected in an increase in the degradation temperature and a degradation rate of 5.3% on day 7. The possibility of tuning the degree of crystallinity, as well as thermal stability and aqueous integrity of thin films of SFW, can be applied to adjust these materials to the requirements of specific biomedical applications.
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