• Title/Summary/Keyword: Solution NMR

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Solubility of Liquid Crystalline Hydroxypropyl Chitin in Organic Solvent (액정성 히드록시프로필키틴의 유기용매에 대한 용해성)

  • Lee, Young Moo;Kim, Seong Soo;Kim, Seon Jeong;Sung, Yong Kiel;Kang, In Kyu;Son, Tae II
    • Applied Chemistry for Engineering
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    • v.4 no.2
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    • pp.403-408
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    • 1993
  • Hydroxypropyl chitin(HPCH) was prepared from chitin by reacting it with propylene oxide. The formation of liquid crystalline character of HPCH was investigated using halogenated organic solvents. Solid state $^{13}C$ NMR spectra for chitin and HPCH confirmed the incorporation of hydroxypropyl moiety. The degree of substitution of HPCH was around 0.8 as detected by elemental analysis. WAXD patterns of chitin and HPCH showed that an incorporation of hydroxypropyl unit in chitin contributed to reducing the crystallinity and enhancing the solubility in organic solvents. Polarized light microscopic pictures of concentrated HPCH solution showed that HPCH formed cholesteric liquid crystalline character at about 25w/v% solution in dichloroacetic acid and 1, 2-dichloroethane. Inherent viscosity of HPCH solution in a mixed solvent showed a transient decrease.

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Study on the characteristics and biodegradable of synthetic PLGA membrane from lactic acid and glycolic acid (젖산 및 글리콜산에서 합성된 PLGA 멤브레인의 특성과 생분해성에 관한 연구)

  • Xie, Yuying;Park, Jong-Soon;Kang, Soon-Kook
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.16 no.4
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    • pp.2958-2965
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    • 2015
  • The PLGA(Poly lactide-co-glycolide) Copolymer have been actively applied to the medical implant material as biomaterials. PLGA membrane was able to alveoloplasty with osteotomy for favorable degradation characteristics and possibilities for sustained drug delivery. In this study, PLGA membrane was prepared using phase inversion method, and examined to optical method analysis(NMR, IR), mechanical property measurement (tearing strength) and thermal characteristic analysis(DSC). In addition, the biodegradation characteristics of the PLGA membrane filled with a PBS(Phosphate Buffered Solution) of the water bath ($60^{\circ}C$) according to the degree of surface degradation in the degradation time, the pH change of the solution and change of the mass of the membrane were measured.

Molecular Dynamics Simulations on β Amyloid Peptide (25-35) in Aqueous Trifluoroethanol Solution

  • Lee, Sang-Won;Kim, Yang-Mee
    • Bulletin of the Korean Chemical Society
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    • v.25 no.6
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    • pp.838-842
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    • 2004
  • Amyloid peptide (A${\beta}$) is the major component of senile plaques found in the brain of patient of Alzheimer's disease. ${\beta}$-amyloid peptide (25-35) (A${\beta}$25-35) is biologically active fragment of A${\beta}$. The three-dimensional structure of A${\beta}$25-35 in aqueous solution with 50% (vol/vol) TFE determined by NMR spectroscopy previously adopts an ${\alpha}$-helical conformation from $Ala^{30}$ to $Met^{35}$. It has been proposed that A${\beta}$(25-35) exhibits pH- and concentration-dependent ${\alpha}-helix{\leftrightarrow}{\beta}$sheet transition. This conformational transition with concomitant peptide aggregation is a possible mechanism of plaque formation. Here, in order to gain more insight into the mechanism of ${\alpha}$-helix formation of A${\beta}$25-35 peptide by TFE, which particularly stabilizes ${\alpha}$-helical conformation, we studied the secondary-structural elements of A${\beta}$25-35 peptide by molecular dynamics simulations. Secondary structural elements determined from NMR spectroscopy in aqueous TFE solution are preserved during the MD simulation. TFE/water mixed solvent has reduced capacity for forming hydrogen bond to the peptide compared to pure water solvent. TFE allows A${\beta}$25-35 to form bifurcated hydrogen bonds to TFE as well as to residues in peptide itself. MD simulation in this study supports the notion that TFE can act as an ${\alpha}$-helical structure forming solvent.

Synthesis and Characterization of Copolyester Sizing Agents

  • Baik, Doo-Hyun;Kim, Gil-Lae
    • Fibers and Polymers
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    • v.2 no.1
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    • pp.148-151
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    • 2001
  • The effect of main chain structure of anion-containing copolyesters on the properties of copolyester sizing agents was investigated. The copolyesters were prepared by conventional two step polymerization technique from DMT, DMI, DMS, EG, and DEG. The copolyesters synthesized were characterized by atomic absorption spectroscopy, $^1$H-NMR Spectroscopy, GC, FTIR Spectroscopy, and DSC. The solubility decreased as the DMT content increased. The copolyesters having DMT:DMI = 1:1 showed the minimum viscosity. The effect of EG content on the solution stability was not clear and the samples having high DMI content showed better solution stability. The water resistance was best when only DMI and EG were used, while it was worst when DMT:DMI was 1:0.

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Radiosterilization of Medical Products(II) (전이방사선을 이용한 의료제품 멸균연구 II)

  • 이강순;천기정;김기수
    • Korean Journal of Microbiology
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    • v.13 no.2
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    • pp.64-70
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    • 1975
  • As a serial experiment of radiosterilization of medical products, we investigated the feasibility of using gamma ray to sterilize antibiotics, tetracycline HCl. Tetracycline HCl in aqueous solution and dried state irradiated with several dose levels was assayed for physico-chemical properties by checking UV absorption spectra, paper chromatogrph. IR spectra and NMR sepctra, and antibiotic activities by [means of agar plaque technique and tube $d_1$]ution method. In physico-chemical propertis and biological activities, the teracycline HCl in dried state remained radioresistant up to exposure of 10 Mrad, however, in aqueous solution, the dose of 300 Krad produced a significant inactivation. From the results of this study, radiosterilization of tetracycline HCl is more recommendable in the dried state than in aqueous solution.

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Optimum Synthesis and Characterization of Precursor Solution for a Hard Coating Silica Film Prepared by Sol-Gel Process

  • Kim, Seon Il;Kim, Gu Yeol;Im, Hyeong Mi;Lee, Bong U;Na, Jae Un
    • Bulletin of the Korean Chemical Society
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    • v.21 no.8
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    • pp.817-822
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    • 2000
  • Crack-free hard coating siIica films were prepared by sol-gel processfrom twokinds of silicon alkoxide (tetra-ethoxysilane and methyltrimethoxysilane) and two kinds of alcohol (methanol and isopropyl alcohol) with an acid catalyst,acetic acid. A silicate framework of the precursor solution was investigated by infrared spectros-copy (IR) in the process of hydrolysis and condensation. Theextent of the condensation in the intermediates was elucidated by gel permeation chromatography (GPC) and 29Si-NMR spectroscopy. The hard coating films werecharacterized by IR,scanning electron microscope (SEM), thermo gravimetric analyzer (TGA) and dif-ferential scanning calroimeter (DSC). The synthetic condition for the crack-free and transparent silica film for-mation was optimized interms of starting materials for the precursor solution as well as preparation method of the silica film.

Characterization of Fibroin Biosynthesis in the 5th Instar of Bombyx mori (5령 누에에 있어서 Fibroin 생합성의 특성)

  • 이인전;여주홍
    • 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.

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Antioxidative Activity of Flavonoids Isolated from Jindalrae Flowers (Rhododendron mucronulatum Turcz.) (진달래꽃으로부터 분리된 플라보노이드 화합물의 항산화성에 관한 연구)

  • Kim, Mi-Ae;Jones, A. Daniel;Chung, Tae-Yung
    • Applied Biological Chemistry
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    • v.39 no.4
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    • pp.320-326
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    • 1996
  • Seven antioxidative flavonoids were isolated from Jindalrae flowers (Rhododendron mnonulatum Turcz.), an edible plant in Korea. These compounds were identified as afzelin, ampelopsin, catechin, myricetin, myricitrin, quercetin and quercitrin on the basis of IR, UV, FAB-MS, $^1H\;NMR,\;and\;^{13}C\;NMR$ data. These compounds were consisted of two flavonols, three flavonol glycosides, a flavane, and a dihydroflavonol. The flavonol glycosides (14.4 g) present in th ethyl ether and ethyl acetate fractions comprised up to 82% of their total flavonoid amount (17.6 g) finally recovered by means of polyamide C-200 column chromatography, preparative TLC, recrystallization, and Sephadex LH-20 column chromatography. The antioxidant activities were measured in an ethanol solution of linoleic acid in the presence of ferric thiocyanate. The antioxidant efficiency increased in the order of afzrlin<$\alpha-tocopherol$

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Flavonoidal constituent in Korean Lactuca dentata Makino (한국산 씀바귀의 Flavonoid 성분에 관한 연구)

  • Chung, Kang-Hyun;Yoon, Kwang-Ro;Kim, Jun-Pyong
    • Journal of the Korean Society of Food Culture
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    • v.9 no.2
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    • pp.131-136
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    • 1994
  • The ethylacetate extract of Lactuca dentata Makino showed 6 flavonoidal components as detected by ferric chloride solution. The flavonoidal constituent of Lactuca dentata Makino was isolated and purified by the series of column chromatography. The chemical structure of one of the flavonoidal component named as compound E was identified by UV, IR and NMR spectrometry. The melting point range of compound E was $249.5^{\circ}C-251^{\circ}C$. The UV and IR spectra of purified compound E, and its genin were measured with the various shifting agents. The results of UV analysis showed the free state of hydroxy group at 3rd and 4th carbon and binding of sugar at the 7th carbon of compound. The sugar bound to the compound E was identified as glucose by TLC. The IR spectrum showed the presense of hydroxy group, conjugated carbonyl group and aromatic group. The analysis of NMR spectrum was done to the purified compound and its derivatives. The chemical shifts against hydrogen atom, hydroxy group, and the moiety of luteolin were observed in the NMR spectrum along with their position and number as well as type of sugar bound. The isolated and purified compound was identified as $luteolin-7-0-{\beta}-D-glucoside$.

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Synthesis and Supramolecular Assembly of Ru(II)-Terpyridine Complexes linked with β-Cyclodextrin or Adamantyl Group (β-CD 또는 아다만탄이 결합된 루테늄(II)-터피리딘 착화합물의 제조와 초분자 조립)

  • Park, Dae-Rim;Chung, Yong-Chae;Choi, Kyung-Ho;Kim, Hyung-Jin
    • Journal of the Korean Chemical Society
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    • v.51 no.6
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    • pp.526-535
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    • 2007
  • Ru(II)-terpyridine complexes (8, 9, 11) linked with adamantyl or β-cyclodextrin moieties were synthesized and characterized based on their 1H and 13C NMR spectra as well as MS spectra. Ru(II)-terpyridine complexes (8, 11) linked with adamantyl moiety were readily dissolved in aqueous solution via encapsulation by β-cyclodextrin when they were mixed with an equimolar amount of β-cyclodextrin. In the similar way, the adamantane guest of the Ru(II)-terpyridine complexes (8, 11) were encapsulated by β-cyclodextrin moiety of the ruthenium complex 9 to afford supramolecular assemblies in aqueous environment. Formation of assemblies was corroborated by 1H NMR spectroscopy.