• Fibers and Polymers
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• v.7 no.4
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• pp.333-338
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• 2006

Silk fibroin (SF) fiber from the Antheraea pernyi silkworm was treated with a 1.23 N iodine-potassium iodide ($I_2-KI$) aqueous solution, and the structure and physical properties were investigated to clarify the effects of the iodine treatment. The noticeably high weight gain value of SF fiber, about 25 wt% was attributed to the absorption of polyiodide ions in the form of $I_3{^-}\;and\;I_5{^-}$. Fourier transform infrared spectroscopy and X-ray diffraction measurements suggested that polyiodide ions mainly entered the amorphous region. In addition, a new sharp reflection on the meridional direction, corresponding to a period of $7.0{\AA}$, was observed and indicated the possibility of the formation of mesophase structure of ${\beta}$-conformation chains. Dynamic viscoelastic measurements showed that the damping tan ${\delta}$ peak at $270^{\circ}C$ gradually shifted to lower temperature in the iodinated SF fibers, suggesting an enhancement of the molecular motion of the fibroin chains induced by the presence of polyiodide ions. With heating above $254^{\circ}C$, the iodine component introduced intermolecular cross-linking of SF, and the melt flow of the sample was inhibited. The thermal decomposition stability of fibroin molecules was greatly enhanced by iodine treatment.

• International Journal of Industrial Entomology and Biomaterials
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• v.45 no.1
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• pp.12-16
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• 2022

Di-tyrosine photo-crosslinking of silk fibroin (SF) is recently highlighted as a biocompatible hydrogel fabrication process, because this method does not need potentially harmful chemical species. However, the resulting crosslinking density is often insufficient to obtain a mechanically stiff hydrogel unless additional oxygen is provided during the reaction. In this study, we proposed a combinational crosslinking method to form an SF hydrogel via the di-tyrosine photo-crosslinking with riboflavin (photoinitiator) and physical interaction of SF chains. In the UV light-irradiated SF solution, small particles formed and these particles promoted β-sheet formation of SF molecules, resulting in quick gelation. The di-tyrosine photo-crosslinking produced nuclei that might trigger regular assembly of SF molecules in high temperature condition. Conclusively, this process would contribute to a development of biocompatible hydrogel fabrication for biomedical uses of SF hydrogels.

• Journal of Sericultural and Entomological Science
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• v.51 no.1
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• pp.15-19
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• 2013

Antheraea pernyi silkworm is one of typical wild silkworms, which spins a tawny color cocoon. The cocoon has been used as a resource for textile material due to strong chemical stability and good mechanical properties. In this study, to increase the solubility efficiency of A. pernyi silk fibroin, the composition of dissolution solvent were examined. Calcium chloride tertiary system, normally used for dissolution of Bombyx mori silk fibroin, does not act on A. pernyi silk fibroin. Calcium nitrate system dissolves A. pernyi silk fibroin, and calcium nitrate ethanol system do more easily than calcium nitrate system. Amino acid composition of A. pernyi silk fibroin obtained after dissolution is mainly composed of alanine, glycine, and serine. A. pernyi silk fibroin would be used for non-textile applications near future.

• Journal of Sericultural and Entomological Science
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• v.44 no.2
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• pp.87-92
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• 2002

Dissolution of Antheraea pernyi silk fiber was carried out in a zinc chloride solution with various dissolving conditions. The solubility was significantly dependent on the concentration of zinc chloride, dissolving temperature and time. The proper conditions of dissolution were found as 8 M zinc chloride, 70$^{\circ}C$ temperature and 30 min dissolving time. Regenerated A. pernyi silk fibroin powder was obtained through dialysis. FTIR and XRD showed that regenerated A. pernyi silk powder was composed of a ${\beta}$-sheet as well as an ${\alpha}$-helix conformation.

• Journal of Sericultural and Entomological Science
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• v.43 no.1
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• pp.49-52
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• 2001

The collagen growth effects in rats using B. mori fibroin sponge sheet, pure fibroin solution and chitosan sponge sheet were investigated. Histopathological inspection of the wound 12 days later showed the increse of a vascular ingrowth and the absence of inflammatory cells. Wound healing effects were accelerated in the order of Fibroin sponge sheet$\geq$Fibroin dressing solution〉Chitosan sponge sheet〉Control. The mean percentage of collagen production in rats after 12 days was 46.12$\pm$4.58% and 42.11$\pm$5.67% in fibroin sponge sheet and dressing solution-treated rats, respectively. These values were higher than the relative content in the chitosan sponge sheet and control groups, which was 23.87$\pm$3.24 and 2.42$\pm$0.32%, respectively.

• International Journal of Industrial Entomology and Biomaterials
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• v.22 no.1
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• pp.5-10
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• 2011

The effect of sample handling condition on the rheological measurement of regenerated silk fibroin formic acid solution using parallel plate geometry was investigated. In case of loading method, the loading by pouring sample solution resulted in the best reproducibility of rheological measurement. Loading with spoon showed a high variance of viscosity value at low shear rate region ($0.01{\sim}1sec^{-1}$) while loading with syringe exhibited a low reproducibility of viscosity at high shear region ($1{\sim}100sec^{-1}$) with a disappearance of shear thinning phenomenon. It was revealed that the sample loading with small extra amount lead to the most reproducible result. The sample loading with the exact amount for the measuring plate resulted in a lack of reproducibility of high shear viscosity, while the loading with large extra volume produced a limited consistency of low shear viscosity. It was turned out that 3 min. of waiting time before measurement was the optimum condition for reliable result. When the waiting time was less than 1 min., the low shear viscosity was obtained with a lack of consistency. On the other hand, the sample solution started drying when the waiting time increased up to 5 min.

• International Journal of Industrial Entomology and Biomaterials
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• v.6 no.2
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• pp.151-155
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• 2003

Using gel filtration chromatography, high molecular silk fibroin with high purity was obtained and silk flbroin microsphere particles (SFMP) could be simply made by spray dryer method. Also, some of the physicochemical properties of SFMP and morphology were investigated. The average molecular weight of pure silk fibroin protein dissolved in calcium chloride is about 61,500g/㏖ as measured by gel permeation chromatography. SFMP was spherical in shape, and particles, sized average of 2 ${\pm}$ 10 ${\mu}$, were observed by SEM and particle analyzer, respectively. Obtaining microspheres particles by spray dryer method accelerated the transition from the random coil to the $\beta$-sheet structure during spray dryer treatment. It was identified by the basic fourier transform infrared spectroscopy of SFMP. The swelling ratio of SFMP is majorly dependent on the pH of the solution, not on the occurred gelation. The characteristic structure, which might be applicable to immobilization of drugs is superior to other matrix materials for the use of biomaterials with skin affinity.

• Polymer(Korea)
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• v.29 no.4
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• pp.408-412
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• 2005

Structure and characteristic of the films blended chitosan matrix with silk fibroin, extracted from Bombyx mori, were studied by X-ray diffraction, differential scanning calorimetry, FT-IR spectra analysis, SEM photographs, contact angle measurement and water absorbency in order to use as biomaterials. The blend films of $0\~30 wt\%$ fibroin content were prepared in acetic solution with $Li^+$ ion. It was found that the crystallinity of chitosan/fibroin blend films was decreased by the presence of intermolecular interactions such as hydrogen bonding between animo groups of chitosan and carbonyl groups of fibroin. As the proportion of fibroin in the blend increased, anhydrous crystalline phase of chitosan disappeared, and hydrated crystalline phase decreased, and $\beta$-structure crystalline phase of fibroin was formed. Therefore the blend films were crystallized into two different crystalline region of chitosan and fibroin. Surface hydrophilicity and water absorbency increased with blending fibroin. Above 20 $wt\%$ fibroin content, hydrogel film was formed. The surface and section of the film showed uniform microstructure on SEM photographs.

• Journal of Sericultural and Entomological Science
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• v.38 no.2
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• pp.180-185
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• 1996

Biosynthesis tracing of the silk fibroin in Bombyx mori silkworm was examined in vivo with isotopic [1-13C] Gly. labeling by nuclear magnetic resonance method. The [1-13C] Gly. labeled silk fibroin yielded very sharp 13C NMR signal in the posterior silk gland as well as in aqueous solution and the amound of [1-13C] Gly. labeled signal in the silkworm increased gradually and rapidly to 5-th day of fifth instar. However, the decomposition or decrease of the [1-13C] Gly. labeled signal occured from 5-th to 9-th day of fifth instar unexpectedly. These findings suggest that a relative amount of ${\alpha}$-helical portion or amorphous silk II portion was formed without any further signal from 6-th day of fifth instar to pupation. Through peak separation of orientation spectrum, between the fiber axis and the molecular bond direction, N-H bond in Bombyx mori silk fiber as well as the orientation distribution around the silk fibroin axis were determined and two kinds of peaks were also obtained from this orientation spectrum.

• Analytical Science and Technology
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• v.27 no.1
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• pp.27-33
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• 2014

This study described about preparation of the cross-linked silk fibroin (SF) film by ${\gamma}$-irradiation of the casted SF film, which is fabricated from aqueous solution regenerated via fibers of cocoons and their application as supports for human cell culture. The properties of cross-linked SF film were evaluated by FT-IR spectroscopy, contact angle, solubility to water, thermal analysis, surface area analyzer, and morphology via scanning electron microscopy (SEM). The cross-linked SF films were not dissolved in water and exhibited the rough surface morphology, large surface area, and good thermal properties. The human fibroblast cell (CCD-986sk) and embryo kidney-ft cell were well growed on the surface of cross-linked SF film supports prepared by ${\gamma}$-irradiation. The cross-linked SF film prepared by ${\gamma}$-irradiation can be used as biomaterials for human cell culture.