• Journal of Biomedical Engineering Research
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• v.43 no.4
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• pp.251-258
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• 2022

Silk fibroin microparticles were fabricated using a phase separation technique between silk fibroin solution and polyvinyl alcohol. We found that the concentration of polyvinyl alcohol determines the size of microparticles. The mean diameter of the silk fibroin microparticles varied from 3.48 ㎛ to 4.05 ㎛. The silk fibroin microparticle size increased as a function of the concentration of PVA in aqueous silk solution. The resulting silk fibroin microparticles have narrow size distribution (i.e. monodisperse) and smooth/spherical surface. Also, we studied the effects of mouse serum, sodium phosphate buffer (PBS), and pH on the stability of the silk fibroin microparticles. Overall, we demonstrated the simple method to fabricate and to control the silk fibroin microparticles that makes our silk microparticles to be usable for a potential drug delivery carrier.

• Journal of Sericultural and Entomological Science
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• v.37 no.2
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• pp.142-153
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• 1995

This study is undertaken to investigate proper condition and dissolution method of silk fibroin to use it functional material as powder or membrane. Silk fibroin was dissolved with calcium chloride ethanol aqueous solution and hydrochloric acid. When silk fibron was dissolved with calcium chloride ehanol aqueous solution, main chain of silk fibroin was degradaded and molecular conformation was changed. Silk fibroin powder was made from silk fibroin solution. It showed lower thermal decomposition temperature and crystallinity than those of native silk fibroin. And Its molecular conformation was random coil structure. By acid gydrolysis, main chain of silk fibroin was attacked randomly. Silk fibroin powder from hydrolysate showed high crystallinity and thermal decomposition temprature. $\beta$-form molecular conformation was found by IR and X-ray diffraction. Silk fibroin powder form dissolved part with hydrochloric acid showed low thormal decomposition temperature but high crystallinity. During acid hydrolysis, transition of molecular structure of silk fibroin occurred, and it changed to $\alpha$-helix. Silk fibroin film was achieved by casting silk fibroin solution by ehanol solution or saturated vapor treatment, and its molecular conformation changed to $\beta$structure.

• Journal of Sericultural and Entomological Science
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• v.42 no.1
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• pp.42-47
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• 2000

Structural and thermal characteristics of silk fibroin/poly(2-hydroxyethyl methacrylate)(PHEMA) blend films were investigated using FTIR, X-ray diffractometer, differential scanning calorimeter, thermogravimeter and scanning electron microscope. FTIR spectra showed that the conformation of silk fibroin prepared by dissolving in formic acid was $\beta$-sheet, which did not affected by blending with PHEMA. The X-ray diffraction patterns also showed that individual crystalline structure of silk fibroin and PHEMA was not affected for the blend films. The initial thermal decomposition temperature of silk fibroin/PHEMA blend film tends to be higher than either of silk fkbroin or PHEMA. Thermal stability of both polymers, more notably PHEMA, can be improved by blending two components. As a result of SEM observation, the phases separation for silk fibroin/PHEMA blend films occured regardless of blend ratio ; continuous and dispersed phase were silk fibroin and PHEMA component, respectively.

• The Korean Journal of Food And Nutrition
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• v.9 no.4
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• pp.496-499
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• 1996

In order to develop the functional diet food, characteristics of chitosan and silk fibroin composite was designed. Chitosan extracted from a prawn and silk fibroin was prepared from silkworm. The silk fibroin was dissolved rapidly in the 8M LiBr at a temperature of more than 4$0^{\circ}C$. Amino acid composition of fibroin composite revealed the same pattern that of native silk fibroin and regenerated silk fibroin. Predominant amino acid of chitosan-fibroin composite contained glycine, alanine, serine, tyrosine, threonine, and glutamic acid in order. According to the basis on the infrared spectrum, chitosan-silk fibroin composite is not distinguished differents composite ratio of chitosan and silk fibroin.

• Journal of Sericultural and Entomological Science
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• v.40 no.2
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• pp.169-175
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• 1998

The morphology of silk fibroin/poly(vinyl alcohol)(PVA)blend films was investigated using optical microscopy and confocal laser scanning microscopy. The effects of blend ratio and molecular weight of silk fibroin and PVA on phase separation were studied. Macro-phase separation occurred for the silk fibroin-rich/poor region whereas micro-phase separation took place for the dispersed/continuous phase, In spite of differences in molecular weight and blend ratio, it is observed that the dispersed phase and continuous one are composed of silk fibroin and PVA component, respectively. As the molecular weight of silk fibroin and silk fibroin content in blend ratio are decreased, the compatibility of blend is increased due to the reduction of micro-phase separation.

• Textile Coloration and Finishing
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• v.6 no.1
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• pp.62-70
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• 1994

Silk fibroin was dissolved in 9.3 M LiBr aqueous solution at 4$0^{\circ}C$ for 1 hour. The dissolved silk fibroin was regenerated by casting the dialyzed solution into the membrane. The freshly prepared silk fibroin membrane was soluble in water and was. mainly consisted of random coil conformation. By the treatments in saturated water vapor at 3$0^{\circ}C$ and in 75% ethanolic aqueous solution (V/V), the insoluble membranes were obtained and the structure and morphology of those were investigated for the structure by means of X-ray diffraction analysis, infrared spectroscopy, thermal analysis. Rheovibron and scanning electron micrograph. Silk II type crystals were obtained by treating amorphous silk fibroin membrane in the random coil conformtion with 75% ethanol solution(V/V). Crystallization to silk II type crystals occured even after a few minutes, and a large number of silk II type crystals were formed after 30 mins. On the other and, the membrane treated in saturated water vapor was composed of the mixtures of silk I and silk II type crystals. A large number of silk I and silk II type crystals were formed after 24 hours. The micro brownian motion in the amorphous regions of silk fibroin membrane started at about 175~185$^{\circ}C$. $\alpha$ dispersion appeared at about 20$0^{\circ}C$ in the amorphous membrane, and at about 22$0^{\circ}C$ in the crystalline membrane. The crystallization of random coil conformation to silkII type crystals occured at about 215$^{\circ}C$. The surface, bottom and cross-section of the membranes were observed by scanning electrom microscope. Fine forms alike spherulites appeared at the surface of crystalline membrane.

• Journal of Sericultural and Entomological Science
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• v.43 no.1
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• pp.41-48
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• 2001

The purification, dissolution and powdering of stained waste silk obtained from weaving and dyeing process were studied for the surface modification of textile fabric and plastic materials. The whiteness of stained waste silk could be improved through degumming and bleaching with sodium hydrosulfite. The water-soluble fibroin solution can be obtained by dissoving the degummed waste silk in a boiling solution of 50% calcium chloride for 60 minutes. The salts and heavy metals contained in fibroin solution were removed by electric dialysis, wool fiber filtration and gel filtration chromatography. The fibroin powder was prepared by using a fine grinder after the alkali treatment for weakening the silk fiber. The fine fibroin powder of particle size around 30 ㎛ was obtained with a ultra fine-mill, while it was finer below 10 ㎛ with a ball-mill. The dissolved or powdered silk was applied to the surface of fabric with addition of the binder (a urethane resin). The moisture content of polyester and nylon fabrics treated with the silk solution was improved due to hygroscopic property of silk. The fine fibroin powder mixed with the binder ws coated on the surface of synthetic film by use of the air pressed sprayer. It was revealed that the hygroscopicity as well as the softness of fibroin powder coated film was much improved. Therefore, it is thought that the fine silk fibroin powder is applicable as an coating agent for the surface modification of plastic and synthetic leather.

• International Journal of Industrial Entomology and Biomaterials
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• v.20 no.2
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• pp.99-105
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• 2010

In this paper, the regenerated silk fibroins were dissolved in LiBr aqueous solution with different dissolution temperature and time, and the effects of the dissolution condition on the regeneration yield, molecular weight, wet spinnability, and electrospinnability of regenerated silk fibroin were investigated. The regeneration yield, molecular weight distribution, and wet spinnability of regenerated silk fibroin were nearly affected by the dissolution temperature and time. However, the electrospinning performance of silk fibroin was influenced by the dissolution condition implying the electrospinning of silk fibroin is more sensitive process than the wet spinning in the range tested in this study. While $25^{\circ}C$ of dissolution temperature resulted in a good electrospinnability of regenerated silk fibroin, the electrospinnability was slightly deteriorated when silk fibroin was dissolved at $60^{\circ}C$ for 6 hours. Also, though the fiber diameters of electrospun silk fibroin produced by the dissolution at $25^{\circ}C$ for 6 hours and 24 hours were 443 and 451 nm, respectively, that at $60^{\circ}C$ for 5 min was reduced to 411 nm. The fiber diameter was more decreased to 393 nm when the dissolution time increased up to 6 hours at $60^{\circ}C$.

• Journal of Sericultural and Entomological Science
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• v.5
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• pp.53-55
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• 1965

This was the report of Hydroxyproline detection in silk fibroin and the obtained results were as followings. 1. Hydroxyproline was analized 25∼75 p.p.m. in specific species silk fibroin. 2. The amino acid was included more in crossed species silk fibroin than in the original species fibroin. 3. The number of amino acids in silk fibroin increased from 18 to 19 kinds.

• Macromolecular Research
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• v.16 no.7
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• pp.604-608
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• 2008

Color dye-doped silk fibroin nanoparticles were successfully fabricated using a microemulsion method. An aqueous silk fibroin solution was prepared by dissolving cocoons (Bombyx mori) in a concentrated lithium bromide solution followed by dialysis. A color dye solution was also mixed with the aqueous silk fibroin solution. The surfactants used for the microemulsion were then removed by methanol and ethanol, yielding color dye-doped silk fibroin nanoparticles, approximately 167 nm in diameter. The secondary structure of the nanoparticles showed a $\beta$-sheet conformation, as characterized by Fourier transform infrared spectroscopy. The morphology of the nanoparticles was determined by field emission scanning electron microscopy, transmission electron microscopy and atomic force microscopy, and their size and size distribution were measured by dynamic light scattering. The color dye-doped silk fibroin nanoparticles were examined by confocal laser scanning microscopy.