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1.
Protein concentration, pH, the types and concentrations of metallic ions, and extensional flow are thought to be important environment parameters affecting the natural spinning process. In this study, we investigate the effects of the types and concentrations of metallic ions (Ca2+, Mg2+, and K+ ions), pH, and silk fibroin concentration on the sol-gel transition and the rheological behavior of a regenerated silk fibroin (RSF) aqueous solution. The results show that with an increase in the silk fibroin concentration, the weak acidic RSF aqueous solutions containing Mg2+ or Ca2+ ions undergo a phase transition to a weak gel state. Moreover, the rheological characterization of RSF aqueous solutions shows a dramatic change, and their apparent viscosities increase by almost three orders of magnitude and approach the apparent viscosity of the native dope in the silkworm gland. By using conventional pressure equipment, we investigate the dry-spinnability of weak gels. Further, we observe that the as-spun fibers exhibit a smooth surface and have inferior mechanical properties. The structure of the as-spun fibers is predominantly in a random coil or Silk I conformation.  相似文献   

2.
The use of silk protein as a biomaterial has been studied for decades. In this study, silk fibroin (SF)/hyaluronic acid (HA) blend scaffolds were prepared by freeze-drying technique. The structure and properties of the blend scaffolds were examined and analyzed. The results demonstrated that the secondary structures of the SF/HA scaffolds were mainly amorphous and β-sheet structures. The pore radius and porosity of the scaffolds decreased with a decrease in the freezing temperature decrease and an increase in the HA ratio. The pore radius and porosity were regulated from 32.22 μm to 290.76 μm and from 74.1 % to 91.15 %, respectively. In vitro, the SF/HA scaffolds could support the fibroblast cell adhesion and proliferation and showed good cytocompatibility. In vivo, the SF/HA scaffolds were implanted into the dorsum of Sprague Dawley rats to evaluate their bioactivity for dermal tissue reconstruction. The vascular-like structures appeared more rapidly in SF/HA scaffolds than that in the PVA group, and a new dermal layer was formed, as determined by histological analysis. The SF/HA porous scaffolds have promise as a dermal substitute.  相似文献   

3.
Ultra fine fibers were electrospun from regenerated silk fibroin/formic acid solution. Effect of some process parameters on the morphology, diameter and variation in fiber diameter of electrospun fibers were experimentally investigated. Scanning electron microscope was used for the measurement of fiber diameter. Fibers with diameter ranging from 80 to 210 nm were collected depending on the solution concentration and the applied voltages. Response surface methodology (RSM) was used to obtain a quantitative relationship between selected electrospinning parameters and the average fiber diameters and its distribution. It was shown that concentration of silk fibroin solution had a significant effect on the fiber diameter and the standard deviation of the fiber diameter. Applied voltage had no significant effect on the fiber diameter and its standard deviation.  相似文献   

4.
Sodium alginate (SA) and krill protein (AKP) were blended to obtain composite solution, and functional SA/AKP composite fibers were prepared via wet spinning. To further improve the salt tolerance, SA/AKP composite fibers were modified with copper sulfate aqueous solution as secondary coagulation bath because of the strong adsorption to copper ions. The CSA/AKP composite fibers with high salt tolerance have been successfully prepared. The intermolecular interaction of SA/AKP composite system and the two-order structure of protein in the composite system were characterized by Fourier transform infrared spectroscopy (FT-IR). Besides, the crystallinity, morphology, mechanical properties, salt tolerance and water resistance and thermal stability of SA/AKP composites were investigated respectively. The results showed that the adsorption rate and the adsorption capacity of the composite solution to copper ion were significantly higher than those to calcium ion. Under the effect of secondary solidification by copper sulfate, the β-sheet chain of the composite fibers increased from 41.48 % to 49.21 %, the intramolecular hydrogen bond increased from 38.18 % to 44.26 %, the intermolecular hydrogen bond decreased from 59.84 % to 54.70 % and free hydroxyl slightly decreased. The water resistance of the modified composite fibers was improved by about 22 %; when the swelling time was 25 min, the salt resistance increased by about 150 %; the number of grooves on the surface of the composite fibers obviously increased, and the grooves on the surface of CSA/AKP composite fibers and the fiber section structure were much denser; Meanwhile, copper sulfate had some influence on the crystallization, thermal stability and mechanical properties of the composite fibers.  相似文献   

5.
As a biomaterial, besides excellent biocompatibility and biodegradability, suitable macropores and pores structure should be provided to guide cell extension and migration. In present study, the silk fibroin (SF) scaffold with uniaxial channels was prepared by directional temperature field freezing technique. The average pore diameter, pore density and porosity of the scaffold with oriented channels are ～128.7 µm, ～158 mm?2 and ～91.4 %, respectively. By controlling of the temperature gradient direction, the oriented multichannels of the scaffolds were formed in longitudinal easily. In process of the scaffolds fabrication, the directional growth of ice crystal could shear and draft to the silk fibroin molecule segments, which resulted in the new crystal nucleus formation in new zone and increase of β-sheet components in the scaffolds. In vitro, L929 cells were seeded on the scaffolds with oriented channels to evaluate the effect on cell behavior. Cell viability, adhesion and morphology were determined by methyl thiazolyl tetrazolium, confocal microscope and scanning electron microscope. The results showed that the cells anchored on the oriented channels, spread along the direction of the channels and hold a higher viability on the scaffolds with oriented channels. These new oriented multichannel scaffold could guide the adhesion and proliferation of L929 cells, which hold a potential in tissue engineering.  相似文献   

6.
Herein we report successful synthesis of silk fibroin (SF) three dimensional scaffolds (SF 3D-scaffold) from SF sponge and SF nanofibers. Both the nanofibers and sponge were prepared from Bombyx mori fibroin. The SF 3D-scaffold was prepared by electrospinning the fibroin nanofibers over the sponge. Surface morphology was determined by scanning electron microscopy (SEM), while nanofiber diameter and pore size were measured using imageJ software. Effect of spinning time on the pore size and cell adhesion was determined. Average diameter of the SF nanofibers was measured to be 320 nm and pore size was found to reduce with increasing spinning time, such that, for 1 h spinning time pore size was 231 µm and the same for 3.5 h was 4.1 µm. However, the number of pores increased with spinning time. The results confirmed adhesion of MC3T3-E1 cells on the SF sponge, SF nanofibers and SF three dimensional scaffolds. Higher cell adhesion was found on the three dimensional scaffold in comparison to the nanofibers and sponge, possibly due to highly porous structure with very small and numerous pores in the resultant composite; hence more cell adhesion sites. The cell adhesion result confirmed biocompatibility of the SF 3D-scaffold and hence its suitability for applications in tissue engineering.  相似文献   

7.
We successfully prepared optically transparent silk fibroin-cellulose nanofiber (CN) composite films from solvent casting using a stable CN suspension in an aqueous silk fibroin solution. The transmittance of the silk fibroin composite films was observed by a UV-visible spectrophotometer. The secondary structural change of the silk fibroin caused by the incorporation of CNs was characterized using Fourier transform infrared spectroscopy. A tensile test was carried out to investigate the mechanical properties. The results showed that the composite film exhibited visible-light transmittance of 75 %, and its mechanical strength and Young’s modulus were increased by 44 % and 35 %, respectively, as compared to a neat silk fibroin film.  相似文献   

8.
We studied the key characteristics of a novel silk yarn reeled from fresh cocoons. Compared with traditional silk yarn, this novel silk yarn displayed better mechanical properties, especially in terms of a higher breaking stress and toughness, and exhibited a different surface morphology. A cross-sectional observation and the sericin content results illustrated that different sericin coatings on the silk yarn reeled from fresh cocoons surface did not improve the mechanical properties. The degumming and tensile testing analysis indicated that degummed silk fibroin of novel silk yarn is able to resist deformation and fracture better than silk fibroin of traditional silk yarn. The FTIR results revealed that the selected techniques is an important contributor to the silk fibroin mechanical properties, because novel technique brought higher percentage beta-sheet structures in novel silk yarn fibroin than traditional silk yarn. The new technique that using novel silk yarn has improved its mechanical properties and it is expected that the silk yarn with superior mechanical properties could be used in fabrics transistors, electrodes and reinforced biomaterials.  相似文献   

9.
Enzymatic oxidation of tyrosine side-chains in proteins could produce reactive o-quinones that might subsequently react with the primary amino groups of functional compounds, which provided a worthwhile reference for functionalization of fibrion materials. In the present work the potential for using tyrosinase to graft the bovine lactoferrin onto Bombyx mori silk fibroin was examined. Lactoferrin could adsorb onto silk fibers and covalently bind to the previous enzymatically oxidized fibroin surface. The enzyme-generated quinones in silk fibers also might cause self-crosslinking of fibroin peptides, which led to beneficial changes of silk properties. For the fabric treated with tyrosinase and lactoferrin slight improvements of dyeability and strength were obtained in comparison to the control. The combinedly treated fabric showed encouraging resistance to S. aureus and E. coli, the antibacterial activities reached to 87.0 % and 76.4 %, respectively. The durability of the antibacterial silk was noticeably higher than that of the sample treated with lactoferrin alone.  相似文献   

10.
Regenerated silk fibroin(SF)/Poly(vinyl alcohol)[PVA] blend films were prepared using different casting solvents, water and formic acid, to elucidate the effect of casting solvent on the structure and miscibility of SF/PVA blends. FTIR and XRD measurement suggested thatβ-sheet conformation of SF was not changed by addition of PVA in case of formic acid casting and the casting solvent determined the crystallized component of SF/PVA, leading to a different trend in the overall crystallinity between the two blends. The casting solvent had a dominant role in deciding phase behavior and molecular miscibility of blend films. SEM observation and DMTA measurement elucidated that water solvent produced phase-separated blend films while formic acid yielded one phase blend films with partial miscibility in molecular level indicating that the miscibility of SF blend can be improved by choosing a proper co-solvent.  相似文献   

11.
This article describes a new process for strengthening natural silk fibers. This process is simple yet effective for mass production of high strength silk fibers, enabled by drawing at a lower temperature and immediately heat setting at a higher temperature. The processing conditions were investigated and optimized to improve the strength. Silk fibers drawn to the maximum ratio at room temperature and then heat set at 200 °C show best tensile properties. Some salient features of the resulting fibers are tensile strength at break reaching 533±10.2 MPa and Young’s modulus attaining 12.9±0.57 GPa. These values are significantly higher than those of natural silk fibers (tensile strength increased by 44 % and Young’s modulus by 135 %). Wide-angle X-ray diffraction and FTIR confirm the transformation of silk I to silk II crystalline structure for the fiber obtained from this process. DSC and TGA data also provide support for the structural change of the silk fiber.  相似文献   

12.
Silk grafting with chitosan and crosslinking agents   总被引：2，自引：0，他引：2  
Chitosan grafting onto silk was tested with three crosslinking agents: trifunctional epoxy resin Araldite DY-T, PEG400 dimethacrylate, and glutaraldehyde in acetic as well as in tartaric acid solutions. Operating conditions were studied to obtain a significant silk weighting with satisfactory graft yields. With the epoxy crosslinker the weight gain was in the range from 1.8 to 8.8 % with graft yield from 8 to 23 %. In the case of PEG400DMA weight gain was 8–12 % with 22–24 % graft yield. With glutaraldehyde in tartaric acid solution a maximum weight gain of 8.4 % with 27.6 % graft yield was obtained. Results of determination of primary amino groups on the grafted silk showed that with epoxy and glutaraldehyde, unlike PEG400DMA, the amino groups of chitosan were only partially involved in crosslinking. Results of DSC analyses suggested that the modification of fibroin structure in chitosan-grafted silk was stronger with glutaraldehyde than with epoxy or dimethacrylate. FTIR-ATR spectra of grafted fibers were found very similar to that of control silk with an additional weak peak ascribable to chitosan in 1180–1080 cm−1 range. Surface investigation through AFM showed clear morphology differences between chitosan-grafted silk with epoxy or dimethacrylate and that crosslinked with glutaraldehyde; the latter appears uneven and scale-like, the others slightly rougher than the original silk.  相似文献   

13.
Fourier transform infrared (FTIR) and solid state13C NMR spectroscopic methods were used to investigate changes in maize and sorghum proteins on wet cooking and popping. FTIR spectra indicated that wet cooking led to proteins in two normal sorghums, namely NK 283 (a red hybrid) and KAT 369 (a white variety), two sorghum mutants (P850029 and P851171) and a maize hybrid (PAN 6043) assuming more antiparallel intermolecular β-sheet character, possibly at the expense of some α-helical conformation. Solid state13C NMR, using the technique of Cross Polarisation Magic Angle Spinning showed shifts of the protein carbonyl carbon and α-carbon resonances upfield on wet cooking in all samples, also indicating a change in protein secondary structure from α-helical to β-sheet conformation. The extent of secondary structural change on wet cooking seemed to be greater in sorghum than in maize and may have a bearing on the inferior protein digestibility of wet cooked sorghum compared to maize. Popping produced the same secondary structural change as observed for wet cooking in both sorghum and maize. However, the extent of change on popping was less than on wet cooking in sorghum and maize.  相似文献   

14.
The tussah silk fibroin (TSF) nanofibers with 611 nm diameters were prepared by electrospinning with the solvent hexafluoroisopropanol (HFIP). And then, the TSF nanofibers were crosslinked by 1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide/N-Hydroxysuccinimide (EDC/NHS) crosslinking agent. The morphology and microstructure of the crosslinked TSF nanofibers were characterized by scanning electron microscopy (SEM), Fourier transforms infrared analysis (FTIR), X-ray diffraction, Instron electronic strength tester, and cell culture. After treatment with EDC/NHS crosslinking agent, the TSF nanofibers swelled and its average diameter increased from 611 to 841 nm. FTIR and X-ray diffraction results demonstrated that random coil, ??-helix, and ??-sheet co-existed in the TSF nanofiber mats, but the content of ??-sheet increased from 25.26 to 45.34 %, and the random coil content decreased from 32.47 to 24.94 %. Compared with the electrospun pure TSF nanofiber mats, the crosslinked TSF nanofiber mats exhibited a lower breaking tenacity and initial modulus, which were 5.51 MPa and 9.86 MPa, respectively. At the same time, the extension at break of the crosslinked TSF nanofiber achieved 109.38 %. In cell culture evaluation, the crosslinked TSF nanofibers were found to support cell adhesion and spreading fibroblast L373 and bone marrow mesenchymal stem cells (BMSCs), which had potential utility in a range of tissue engineering.  相似文献   

15.
This paper describes how coloration of silk can be achieved using a coupling reaction between a diazonium compound, made from Color Base Red G (C.I. 37105) and tyrosine residues in the silk protein fibroin. A pigment with an azo structure obtained from the reaction between the diazonium of Color Base Red G with p-methylphenol was synthesized and studied as a model compound for the coloration reaction. The colored materials were characterized using UV-vis, FT-Raman, FT-IR, 1H-NMR, and mass spectroscopy. Both the colored silk and the model compound gave yellow colors with absorption maxima in the region of 400 nm. The results suggest that the use of coupling reactions could be developed into a dyeing method for protein fibers or other protein materials that contain tyrosine residues. Because the chromophores are incorporated into the protein chains, such dyed silks should have good wet fastness properties.  相似文献   

16.
Consolidation of fragile historic silks is of great importance for further displays and researches. An effective and convenient method to consolidate aged silk fabric has been proposed by using a silk fibroin (SF)/ethylene glycol diglycidyl ether (EGDE) consolidation system. Artificial aged silk fabrics treated with SF/EGDE show great improvement in mechanical properties. The chemical reaction between EGDE and silk fabrics has been proved in previous paper. And in this paper, mechanical test, field emission scanning electron microscopy (FESEM), Fourier transform infrared spectrum (FTIR) test and amino acid analysis (AAA) were applied to illustrate the interactions between SF and silk fabric, EGDE and SF. Results show that SF takes part in the consolidation in the form of adhesions on the surface of silk fibers. The chemical reactions and film adhesion are both responsible for the improvements of mechanical properties in the consolidation.  相似文献   

17.
Cellulose nanowhisker (CNW) reinforced electrospun Bombyx mori silk fibroin (SF) nanofibers were fabricated. The morphology, structure, and mechanical properties of nanofibers were investigated by FE-SEM, TEM, FTIR, and tensile testing. It was found that the nanofiber size decreased obviously from 250 nm in the unreinforced mat to 77–160 nm in the CNW reinforced mats depending on the CNW content due to the increased conductivity of spinning dope. In the reinforced mats, the CNWs were embedded in the SF matrix separated from each other, and aligned along the fiber axis. There was a positive correlation between the CNW content and the tensile strength and Young’s modulus of reinforced mats. However the strain at break dropped gradually with the increase of CNW. When the CNW content was 2 w/w%, the tensile strength and Young’s modulus of reinforced SF nanofiber mats were about 2 times higher than those of unreinforced mat.  相似文献   

18.
Silk is very promising in the field of biomaterials as a natural biomacromolecule. Silk protein can be made into various forms of materials, including hydrogels. However, silk protein-based hydrogels have not attracted much attention due to its weak mechanical properties. Here, we report high water content silk protein-based hydrogels with tunable elasticity which were fabricated through Ru(II) mediated photochemically cross-linking tyrosine residues in regenerated silk protein. The regenerated silk protein was characterized by Fourier transform infrared spectroscopy (FTIR). The gelation kinetics of the silk protein was studied by rheology measurements. The compressive mechanical properties of the silk protein-based hydrogels was investigated using compressive tests and dynamic mechanical analysis (DMA). Compressive modulus of the hydrogels reached 349±64 MPa at 15 % strain. The fabricated silk protein-based hydrogels were also characterized by Scanning electron microscopy (SEM), revealing an interconnected porous network structure, typical of hydrogels, with an average pore size of approximately 130 μm. Finally, biocompatibility of the silk protein-based hydrogels was demonstrated through cell culture studies using a human fibroblast cell line, HFL1. The reported silk protein-based hydrogels represent a promising candidate for biomaterial applications.  相似文献   

19.
Different shapes of dispersed phase such as sphere, laminar and fibrillar can form in the matrix phase of polymer blends. Production of blend fibers in melt spinning process can result more effective in fibrillar phase morphology formation than in other processes. In this research, the matrix-fibril morphology development during the melt spinning of polypropylene/poly(butylenes terephthalate) was studied. The shapes of blend dispersed phase collected from different zones of the melt spinning line were evaluated by scanning electron micrographs (SEM) and rheological mechanical spectra (RMS). The results showed that fibrillar shape could not be created in the PP/PBT blend fiber samples exited from the spinneret orifice (gravity spun fibers) at low contents (5 percent) of the PBT dispersed phase. However, a complete fibrillar structure was formed in all the as-spun PP/PBT blend fiber samples (melt drawn). The rheological evaluations confirmed a network structure resulting from fibril formation for the samples with high contents (20–40 %) of the PBT dispersed phase and the formation of spherical shape with low contents (5–10 %) of the PBT dispersed phase in matrix of the blend fibers. It was observed that the flow fields of processing zones and blend ratio, in producing the blend fibers, have intensive effects on morphological variations; besides there was a strong relation between the mechanical and morphological properties.  相似文献   

20.
Biodegradable polymer was prepared as thermoplastic starch (TPS). Due to poor mechanical properties and high water absorption of TPS, thermoplastic rice starch (TPRS) was modified by reinforcing with natural silk protein fibers, as an alternative choice of fiber reinforcement. Different contents and lengths of silk fibers were varied and used as the reinforcement. Internal mixer and compression molding machine were used to mix and shaped the TPRS/silk composites. It was found that stress at maximum load and Young??s modulus of the TPRS/silk composites significantly increased with the incorporation of silk fibers. Water absorption of the TPRS/silk composites was also dropped by the addition of silk fibers. Moreover, thermal degradation temperatures of the TPRS/silk composites shifted to higher temperatures by the inclusion of the silk fibers. Functional group analysis and X-ray diffraction patterns were analyzed by FI-IR and XRD techniques, respectively. Furthermore, color measurement, morphology and biodegradation by soil burial test were carried out for different TPRS/silk composites.  相似文献   

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