• Bulletin of the Korean Chemical Society
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• v.23 no.6
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• pp.914-917
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• 2002

• Macromolecular Research
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• v.12 no.4
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• pp.367-373
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• 2004

We have developed a rigorous heat treatment method to improve the biocompatibility of chitosan as a tissue-engineered scaffold. The chitosan scaffold was prepared by the controlled freezing and lyophilizing method using dilute acetic acid and then it was heat-treated at 110$^{\circ}C$ in vacuo for 1-3 days. To explore changes in the physicochemical properties of the heat-treated scaffold, we analyzed the degree of deacetylation by colloid titration with poly(vinyl potassium sulfate) and the structural changes were analyzed by scanning electron microscopy, Fourier transform infrared (FT-IR) spectroscopy, wide-angle X-ray diffractometry (WAXD), and lysozyme susceptibility. The degree of deacetylation of chitosan scaffolds decreased significantly from 85 to 30% as the heat treatment time increased. FT-IR spectroscopic and WAXD data indicated the formation of amide bonds between the amino groups of chitosan and acetic acids carbonyl group, and of interchain hydrogen bonding between the carbonyl groups in the C-6 residues of chitosan and the N-acetyl groups. Our rigorous heat treatment method causes the scaffold to become more susceptible to lysozyme treatment. We performed further examinations of the changes in the biocompatibility of the chitosan scaffold after rigorous heat treatment by measuring the initial cell binding capacity and cell growth rate. Human dermal fibroblasts (HDFs) adhere and spread more effectively to the heat-treated chitosan than to the untreated sample. When the cell growth of the HDFs on the film or the scaffold was analyzed by an MTT assay, we found that rigorous heat treatment stimulated cell growth by 1.5∼1.95-fold relative to that of the untreated chitosan. We conclude that the rigorous dry heat treatment process increases the biocompatibility of the chitosan scaffold by decreasing the degree of deacetylation and by increasing cell attachment and growth.

• Korean Journal of Materials Research
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• v.34 no.2
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• pp.85-94
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• 2024

The optimization of deacetylation process parameters for producing chitosan from isolated chitin shrimp shell waste was investigated using response surface methodology with central composite design (RSM-CCD). Three independent variables viz, NaOH concentration (X₁), radiation power (X₂), and reaction time (X₃) were examined to determine their respective effects on the degree of deacetylation (DD). The DD of chitosan was also calculated using the baseline approach of the Fourier Transform Infrared (FTIR) spectra of the yields. RSM-CCD analysis showed that the optimal chitosan DD value of 96.45 % was obtained at an optimized condition of 63.41 % (w/v) NaOH concentration, 227.28 W radiation power, and 3.34 min deacetylation reaction. The DD was strongly controlled by NaOH concentration, irradiation power, and reaction duration. The coefficients of correlation were 0.257, 0.680, and 0.390, respectively. Because the procedure used microwave radiation absorption, radiation power had a substantial correlation of 0.600~0.800 compared to the two low variables, which were 0.200~0.400. This independently predicted robust quadratic model interaction has been validated for predicting the DD of chitin.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.37 no.5
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• pp.359-365
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• 2004

To study the lipid adsorption characteristic of chitosans with different molecular weights and the degrees of deacetylation, in vitro test and near-infrared (NIR) spectroscopic analysis have been performed for the measurement of lipid adsorption characteristics of chitosan. The degrees of deacetylation in chitosans were $70{\%},\;85{\%}\;and\;92{\%}$ at different deacetylation times (1 hr, 2 hrs, 3 hrs), respectively. The molecular weight of each chitosan was controlled by enzymatic hydrolysis, and then the molecular weight of the chitosan was 4 kDa. The bulk density, water holding capacity and fat binding capacity of each chitosan powder were $96.2-504.0{\%},\;374.4-1217.9{\%},\;and\;307.0-659.3{\%}$, respectively. The higher molecular weight of chitosan was exhibited the lower bulk density and the higher water and fat binding capacities. Bindinf capacities of chitosan powders to bile salts, cholesterol and linoleic acid were $41.2-63.3{\%},\;40.8-67.4{\%},\;42.6-72.6{\%}$, respectively. In NIR spectrum of lipid adsorbed chitosan the occurrence static eletronical binding between chitosan and lipid was identified by NIR spectrum peak induced from combination of carboxylic group in lipid and amino group in chitosan. In conclusion, the higher degree of deacetylation and molecular weight of chitosan showed the higher lipid binding capacity and the lipid adsorption of chitosan were occurred by combination of carboxylic group in lipids and amino group in chitosan.

• Textile Coloration and Finishing
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• v.11 no.2
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• pp.55-63
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• 1999

The purpose of this study was to investigate the purification of chitin and chitosan for textile finishing agent from crab shell. Weight loss rate(removing Ca and protein), degree of deacetylation, solubility and MIC(Minimum growth inhibitory concentration) value of chitosan and molecular weight of the treated crab shell were measured. The results of this study were as follows : 1) Weight loss rate(removing Ca) of crab shell treated with HCI increased with the concentration of HCI and treatment time, but it became constant over 60 min. of treatment time. 2) Weight loss rate(removing protein) of crab shell treated with NaOH(0.5N∼2N) increased with the concentration of NaOH and treatment temperature and time, but it became constant above loot of temperature and over 200 min. of treatment time. 3) Degree of deacetylation of chitin treated with NaOH increased with the concentration of NaOH(40∼60％), but molecular weight decreased and thus MIC value increased. 4) Concentration of acetic acid should be above 0.3％ to dissolve chitosan easily. Solubility for chitosan was the highest with formic acid, and the next was acetic acid, hydrochloric acid, lactic acid and sulfuric acid in order.

• The Research Journal of the Costume Culture
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• v.13 no.4 s.57
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• pp.576-588
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• 2005

The effect of chitosan pretreatment on the dyeing of cotton fiber and silk fiber was investigated. However, it has been difficult to evaluate the effect of the chitosan precisely, since the characterization of the molecular weight and effect of the degree of deacetylation were not elucidated for the application. The treatment effect may change diversely since the chitosan solution viscosity differs a lot based on the chitosan molecular weight. In this study, three chitosan specimens, varying in molecular weight, were applied for the fabric pretreatment in order to investigate the effect of chitosan molecular weight. Also, in order to maximize the efficacy of the chitosan, highly deacetylated chitosan specimens, meeting the deacetylation degree of $100\%$, were selected far the application. The air-permeability change according to the chitosan molecular weight change, influence on the mordanting, color change, and wash fastness change were investigated.

• Proceedings of the Korean Fiber Society Conference
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• 2003.10b
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• pp.277-278
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• 2003

키틴은 셀룰로오스와 더불어 자연계에 가장 많이 존재하는 천연고분자(선형다당)로서 $\beta$(1$\longrightarrow$4)-2-deoxy-2-acetamido-D-glucopyranose를 기본단위로 하고, 키토산(chitosan)은 천연적으로는 몇몇 미생물에서 발견되며, 키틴의 탈아세틸화반응(deacetylation)에 의해 생성되는 유도체로서 $\beta$(1$\longrightarrow$4)-2-deoxy-2-amino-D-glucopyranose를 기본단위로 한다는 점에서 상이하다. 하지만 키틴과 키토산은 각 기본단위가 반복된 homopolymer가 아니고 서로 일정 정도의 상대 기본단위를 함유하므로 일종의 공중합체 또는 heteropolymer라고 할 수 있으며, 그 조성비 즉 탈아세틸화도 (degree of deacetylation, 이하 DD)에 따라 키틴과 키티산으로 나누어진다.[1] (중략)

• Food Science and Biotechnology
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• v.14 no.3
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• pp.433-436
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• 2005

Chitosans were obtained with varying deacetylation times using the ${\beta}$-chitin isolated from Todarodes pacificus, and their deacetylation degrees and average molecular weights were determined. Films prepared with the squid chitosans were characterized by estimating their tensile strengths, percent elongations, water vapor permeabilities, degree of swelling, and temperatures of glass transition and thermal decomposition. The results suggest that the squid chitosan films were comparable to common crustacean chitosan films in regard of mechanical, moisture barrier, and thermal properties, although further, multilateral investigations are necessary to make a more definitive conclusion.

• Archives of Plastic Surgery
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• v.38 no.4
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• pp.369-375
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• 2011

Purpose: Many hemostatic agents and dressings have been tested with variable degree of success. Chitosan has a positive charge, it attracts red blood cells, which have a negative charge. Our goal is to test the efficacy of new developed chitosan-based hemostatic materials in providing durable hemostasis in a high-flow arterial wound model. Methods: We compared each group with SD rats motality tests and in vitro blood compatibility test by blood clotting index (BCI). We devided the SD rats into 6 groups (N =15) by type of hemostatic agents. A: 100% nonwoven chitosan (degree of the deacetylation: 90%). B: 50% N-acetylation on nonwoven of chitosan gel (degree of the deacetylation: 50%). C: 60% N-acetylation on nonwoven of chitosan ge (degree of the deacetylation: 40%)l. D: Cutanplast$^{(R)}$. E: HemCon$^{(R)}$ F: Gauze. In vivo test, a proximal arterial injury was created in unilateral femoral arteries of 90 anesthetized SD rats. Each materials was made same size and thickness then applied to the injury site for 3 minutes. In vitro test, we compared each group with BCI in human blood. Results: In vivo test, group A showed lower motality rate of 46% than any other groups, Group B and C showed lower motality rate of 60% than group D and E's motality rate of 66%. In vitro test, BCI of group A ($30.6{\pm}1.2$) and B ($29.3{\pm}1.0$) were showed nearly about group D ($29.1{\pm}1.8$) and E ($27.4{\pm}1.6$). Group C ($37.1{\pm}2.0$) showed higher BCI than group A and B, it means group C decreased blood clotting. Conclusion: In conclusion, this study suggests a newly developed chitosan-based hemostatic materials induced durable hemostasis and increased blood clotting, and are considered as effective biologic hemostatic agents.

• Applied Chemistry for Engineering
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• v.10 no.1
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• pp.19-23
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• 1999

Chitosan was partially degraded by using nitrous acid. The deacetylation degree of chitosan decreased with its degree of hydrolysis. Deacetylation degree of each fraction was less than 50%. The degraded product was fractionated by means of precipitation using aqueous methanol solution or aqueous methanol-acetone solution. The molecular weight of each fraction was distributed between 6000 and 4000, and below 2000 for being precipitated using aqueous methanol solution and aqueous methanol-acetone solution respectively. They had narrow molecular weight distributions, and their polydispersities were less than 1.7. The antibacterial activities for each fraction were evaluated against Bacillus subtilis HB 101 and E. coli PP 2, gram-positive bacteria and gram-negative bacteria, respectively. Fraction B (Mw=5100) showed high antibacteiral activity. All fractions were more active against Bacillus subtilis than E. coli.