• KSBB Journal
• /
• v.24 no.6
• /
• pp.563-569
• /
• 2009

Fibroin is an insoluble structural protein from Bombyx mori. It can be solubilized by dissolving in a hot $CaCl_2$ solution and subsequent dialysis. The aqueous solution is unstable and a transition from aqueous fibroin molecules rich in random coil is undergo to one rich in $\beta$-sheet content, resulting in hydrogelation. However, fibroin gel is so fragile and plastic that its mechanical property should be reformed for various applications. In this report, a semi-solid form of fibroin gel was prepared using glycerol and ethanol and was investigated to analyze their flow properties. A fibroin gel with 80% glycerol showed pseudoplastic and thixotropic properties. The square root of its yield stress varied linearly with fibroin concentration and it extrapolated to zero shear stress at 0.2% fibroin. A fibroin gel with 40% ethanol was shown to be highly thixotropic but its shear-thinning behavior was only observed above a certain level of shear rate. Its pseudoplasticity was restored by a high rate of shear stress.

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

• Fibers and Polymers
• /
• v.2 no.2
• /
• pp.58-63
• /
• 2001

Silk fibroin (SF) was dissolved in calcium chloride/ethanol/water mixture(1/2/8 in mole ratio) at $70^{\circ}C$ for 4h. The dissolved silk fibroin was regenerated by casting the dialyzed solution into films. The films were treated with 50% aqueous solution of methanol for different times, and their antithrombogenicity was evaluated by in vivo tests. In vivo blood tests were made by a method of peripheral vein indwelling suture. It was found that the silk fibroin had a good antithrombogenicity and an absorbability even though the polymer showed foreign body reaction. Finally, the blood compatibilty of silk fibroin films which were subjected to structural change by the methoanl treatment, was examined in connection with their interfacial surface energy, and a correlation between these properties was found to be present.

• 한국생물공학회:학술대회논문집
• /
• 2001.11a
• /
• pp.798-799
• /
• 2001

The intermolecular hydrogen bond between silk fibroin in aqueous solution facilitates gelation of silk fibroin. The dependence of gelation by the concentration of silk fibroin, pH and temperature was investigated. The gelation time of silk fibroin is decreased with increasing the concentration of glycerol and temperature within a limited range. The pH optimum for gelation found out to be 9. Hydrophobic additives were investigated to reduce gelation time.

• Journal of Sericultural and Entomological Science
• /
• v.39 no.1
• /
• pp.67-72
• /
• 1997

As a condition for obtaining the silk I type crystal that has stability and high reproducibility, after dissolving silk fibroin crystalline part (Fcp), the changes of recrystallized crystal structure according to dialytic pH were examined by x-ray diffraction and differential thermal analysis. The Fcp was obtained from the aqueous solution of silk fibroin enzymatic proteolyzed by chymotrypsin. The crystal structure of Fcp showed silk II type. When the Fcp was dissolved by 10M LiBr aqueous solution, the Fcp1 showed the silk II type at pH 9. However, besides the silk II type, the silk I type structure begins to appear at pH 8 and only the silk I type structure was found below pH 6. On the other hand, the Fcp2 that calcium chloride was used in the dissolution found only the silk I type crystal structure below pH8.

• International Journal of Industrial Entomology and Biomaterials
• /
• v.27 no.2
• /
• pp.265-270
• /
• 2013

Dialysis is the rate-limiting step in the preparation of aqueous silk fibroin (SF) solution. However, the traditional practice of dialyzing SF solution for at least 48 h to remove LiBr is not based on empirical evidence. The aim of the present study was to systematically measure LiBr content in SF solutions dialyzed for varying lengths of time and assess the potential toxicity of residual lithium ions in cells. Complete removal of lithium ions was not achieved even after 72 h of dialysis, with a residual lithium ion content in the solution of 22.85 mg/l. SF films prepared from solutions dialyzed for 8 and 24 h had predominantly random coil or b-sheet structures, respectively. The residual lithium had little cytotoxicity in NIH3T3 fibroblast cells, but viability was compromised in cells grown on SF film prepared from solution dialyzed for 24 h.

• Journal of Sericultural and Entomological Science
• /
• v.40 no.2
• /
• pp.131-135
• /
• 1998

Changes of silk fibroin molecular weight was studied by enzymatic proteolysis and reverse reaction of enzymatic proteolysis (plastein reaction) using chromatography, X-ray diffraction and thermal analysis methods. When the treatment of enzymatic proteolysis with $\alpha$-chymotripsin to silk fibroin solution, a precipitate of Fcp fractions was formed. And, this was dissolved in LiBr aqueous solution, the precipitate of PIFcp fractions was obtained again. Fcp and PIFcp fractions showed silk IIand silk Itype structure, respectively. Fcp fractions was about 6,900 in molecular weight, PIFcp fractions obtained by plastein reaction on the precipitate of Fcp fractions increased molecular weight to abort 15,000. The molecular weight of Fcp fractions was increased by plastein reaction, but Fcp fractions almost transited to silk I type crystal. The structure of silk I type of PIFcp fractions was steady identified by X-ray diffraction and thermal analysis. As molecular weight of Fcp fractions was gradually low, PIFcp fractions was become to macromolecule little by little.

• Journal of Sericultural and Entomological Science
• /
• v.46 no.1
• /
• pp.28-31
• /
• 2004

Bombyx mori silk fibroin/hyaluronic acid blend films were prepared by mixing aqueous solution of B. mori silk fibroin and hyaluronic acid. According to the FTIR spectra, no interaction between silk fibroin and hyaluronic acid was found. The conformation of silk fibroin in blend films was changed from random coil to $\beta$-sheet structure by treatment of EDC ethanol solution. Thermal degradation peak of silk fibroin and hyaluronic acid was also not altered by blending each other. The average swelling ratio of silk fibroin/hyaluronic acid blend films was 70. Therefore, silk fibroin/hyaluronic acid blend films might be one of possible wound dressing materials.

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

• Journal of Sericultural and Entomological Science
• /
• v.39 no.2
• /
• pp.169-173
• /
• 1997

The behavior of tyrosine(Tyr.) residue of Bombyx mori silk fiber from yellow fluorescent cocoon has been examined for the dependence of pH in aqueous silk solution under the presence of orange II salt. Through the peak separation of angular dependence of spectral pattern of 15N-Tyr. and [1-13C]-Tyr. between the fiber axis and the molecular bond direction, N-H bond in fiber as well as the orientation distribution around the fiber axis were analyzed. Also, and sericin component was obtained from these angular dependence of oriented spectral pattern. The pH dependence of the 13C NMR chemical shift of B. mori silk fibroin was examined in aqueous solution in the presince of orange II are broad at pH$\geq$7.0. However, these become sharper at pH$\geq$8.0 and remain sharp at higher pH. In these higher pH range, a chemical shift change occurs due to the deprotonation of the Tyr. side group of fibroin. At higher pH. such a hydrophobic cluster is destroyed because of the electrostatic interaction according to the deprotonation of the Tyr-OH group.