• Title/Summary/Keyword: 1D $^1H-NMR$

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The Selective Synthesis of ${alpha}$-Sulfo Long Chain Fatty Acid Monoglyceride ((${alpha}$-술폰 고급 지방산 모노글리세라이드의 선택적 합성)

  • Yun, Y.K.;Jeoung, H.G.;Park, S.S.;Kim, T.Y.;Nam, K.D.
    • Journal of the Korean Applied Science and Technology
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    • v.10 no.1
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    • pp.31-38
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    • 1993
  • Anionic polyolic surfactants, ${alpha}-sulfo$ fatty acids that straight long chain alkyl group has from 12 to 18 hydrocarbon numbers, was synthesized with sulfur trioxide-dioxane complex to good yields. New sodium ${alpha}-sulfo$ long chain fatty acid monoglyceride were obtained by reaction that the ketalificaticn and esterification of glycerol, acetone and ${alpha}-sulfo$ long chain fatty acid and hydrolysis respectively. These reaction products separated by column chromatography and their $R_{f}$ values($R_{f}{\times}100$) were 19, 21, 24 and 26 respectively. These compounds were identified by infrared spectroscopy and $^{1}H$ NMR spectroscopy.

Production of Inulin Fructotransferase(depolymerizing) from Flavobacterium sp. LC-413

  • Cho, Chul-Man;Lim, Young-Soon;Kang, Soo-Kyung;Jang, Kyung-Lib;Lee, Tae-Ho
    • Preventive Nutrition and Food Science
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    • v.1 no.1
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    • pp.121-126
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    • 1996
  • A bacterial strain LC-413, producing extracellular inulin fructotransferase which converts inulin into di-D-fructofuranose dianhydride(DFAIII) and amount of oilgosaccharides, was isolated from soil and pre-sumed as Flavobacteium sp. LC-413. The enzyme production was induced by inulin as carbon source and enhanced by the addition of 0.3% malt extract and 0.2% {TEX}$NaNO_{3}${/TEX} as nitrogen source. The enzyme activity in the culture supernatant reached at the maximum, 78.6units/ml, after 11 hours of cultivation in the medium composition of 1.5% inulin, 0.2% {TEX}$NaNO_{3}${/TEX}, 0.05% {TEX}$K_{2}${/TEX}{TEX}$HPO_{4}${/TEX}, 0.05% {TEX}$MgSO_{4}${/TEX}.7{TEX}$H_{2}${/TEX}O, 0.05% KCI, a trace amount of {TEX}$FeSO_{4}${/TEX}.7{TEX}$H_{2}${/TEX}O, and 0.3% malt ext. at 3$0^{\circ}C$. The oilgosaccharide produced by enzyme reaction from inulin was identified as DFA III by and {TEX}${13}^C${/TEX}-NMR spectrosocpy.

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Syntheses of Polysiloxane-Bridged Dinuclear Metallocenes and Their Catalytic Activities

  • 노석균;김수찬;이동호;윤근병;이훈봉
    • Bulletin of the Korean Chemical Society
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    • v.18 no.6
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    • pp.618-622
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    • 1997
  • The polysiloxane-bridged dinuclear metallocenes $[(SiMe_2O)_n-SiMe_2(C_5H_4)_2][(C_9H_7)ZrCl_2]_2$ (n=1 (7), 2 (8), 3 (9)) have been generated as a model complex for the immobilized metallocene at silica surface by treating the respective disodium salts of the ligands with 2 equivalents of $(C_9H_7)ZrCl_3$ in THF. All three complexes are characterized by $^1H$ NMR and measurement of metal content through ICP-MS. It turned out that the values of ${\Delta}{\delta}=[{\delta}_d-{\delta}_p]$, the chemical shift difference between the distal $({\delta}_d)$ and proximal $({\delta}_p)$ protons, for the produced dinuclear compounds (0.47 for 7, 0.49 for 8, and 0.5 for 9) were larger than the Δδ value of the known ansa-type complex holding the same ligand as a chelating one, that is just the opposite to the normal trend. In order to compare polymerization behavior of the dinuclear metallocene with the corresponding mononuclear metallocene, (Cp)$(C_9H_7)ZrCl_2$ was separately prepared. To investigate the catalytic properties of the dinuclear complexes and mononuclear metallocenes ethylene polymerization has been conducted in the presence of MMAO. The polymerization results display the typical activity dependence on polymerization temperature for all complexes. The most important feature is that the polymers from the dinuclear metallocenes represent enormously improved molecular weight compared with the polymer from the corresponding mononuclear metallocene. In addition, the influence of the nature of the bridging ligand upon the reactivities of the dinuclear metallocenes has also been observed.

The chemical structure of polyphenols isolated from cacao bean and their inhibitory effect on ACE (Cacao bean으로부터 분리된 polyphenol 성분의 화학구조분석과 ACE 저해효과)

  • Chang, Young-Youl;Yim, Moo-Hyun;Lee, Man-Chong
    • Applied Biological Chemistry
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    • v.41 no.1
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    • pp.110-117
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    • 1998
  • Seven kinds of polyphenol compounds having ACE activities were isolated and purified by Sephadex LH-20, MCI-gel CHP-20, ${\um}-Bondapak\;C_{18}$ and Fuji-gel ODS $G_3$ sucessively from cacao bean(Ghana). The chemical structures of each compound were determined and identified using analyzers such as $^1H-NMR$, $^{13}C-NMR$, IR, MS, polarimeter and Elemental Analysis. Inhibition effects of isolated polyphenols on angiotensin converting enzyme (concerned with hypertension) were also observed. The results obtained were as follows,; The compounds isolated and identified were confirmed and determined as compound 1 [(+)-catechin], compound 2 [(-)-epicatechin], compound 3 [procyanidin B-1 : (-)-epicatechin-$(4{\beta}{\rightarrow}8)$-(+)catechin], compound 4 [procyanidin B-2 : (-)-epicatechin-$(4{\beta}{\rightarrow}8)$-(-)-epicatechin], compound 5 [procyanidin B-7 : (-)-epicatechin-$(4{\beta}{\rightarrow}6)$-(+)-catechin], campound 6 (procyanidin B-2,3,3'-O -digallate), compound 7 [cinnamtannin A-2 : (-)-epicatechin-$(4{\beta}{\rightarrow}8)$-(-)-epicatechin-$(4{\beta}{\rightarrow}8)$-(-)-epicatechin-$(4{\beta}{\rightarrow}8)$-(-)-epicatechin]. In the inhibition effect on ACE, procyanidin B-2,3,3'-O-digallate (compound 6) showed a higher value of 94.6% for ACE in $100\;{\um}M$ than other compounds such as (+)-catechin (compound 1), (-)-epicatechin (compound 2), procyanidin B-1 (compound 3), procyanidin B-2 (compound 4), procyanidin B-7 (compound 5) and cinnamtannin A-2 (compound 7) showing 67.9%, 61.9%, 88.6%, 82.5%, 72.2% and 82.3% for ACE, respectively. Inhibition of $4{\beta}{\rightarrow}8$ in coupling bond on the ACE enzyme was more effective than that of $4{\beta}{\rightarrow}6$. Procyanidin containing gallate inhibited more effectively than those containing not any. It was also observed that a lot of hydroxy group in the compounds increased the inhibitory effect.

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Structural Change in Transmembrane Region of Syndecan-4 by Mutation

  • Choi, Sung-Sub;Kim, Ji-Sun;Jeong, Ji-Ho;Kim, Yongae
    • Journal of the Korean Magnetic Resonance Society
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    • v.20 no.4
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    • pp.129-137
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    • 2016
  • Transmembrane(TM) proteins are closely related to transport, channel formation, signaling, cell to cell interaction, so they are the crucial target of modern medicinal drugs. In order to study the structure and function of these TM proteins, it is important to prepare reasonable amounts of proteins. However, their preparation is seriously difficult and time-consuming due to insufficient yields and low solubility of TM proteins. We tried to produce large amounts of Syndecan-4 containing TM domain(SDC4-TM) that is related to the wound healing and tumor. Also, mutated SDC4-TM was studied to investigate structural change by modification of dimerization motif. We performed the structure determination by the Polarity Index at Slanted Angle (PISA) wheel pattern analysis based on $^{15}N-^1H$ 2D SAMPI-4 solid-state NMR of SDC4-TM and computational modeling using Discovery Studio 2016.

Overexpression and Spectroscopic Characterization of a Recombinant Human Tumor Suppressor p16INK4

  • Lee, Weon-Tae;Jang, Ji-Uk;Kim, Dong-Myeong;Son, Ho-Sun;Yang, Beon-Seok
    • BMB Reports
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    • v.31 no.1
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    • pp.48-52
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    • 1998
  • $p16^{INK4}$, which is a 16-kDa polypeptide protein, inhibits the catalytic activity of the CDK4-cyclinD complex to suppress rumor growth. Both unlabeled and isotope-labeled human tumor suppressor $p16^{INK4}$ protein were overexpressed and purified to characterize biochemical and structural properties. The purified p16 binds to monomeric GST-CDK4 and exists in a monomer conformation for several weeks at $4^{\circ}C$. The circular dichroism (CD) data indicates that p16 contains high percentage of ${\alpha}$-helix and that the helix percentage maximized at pH value of 7.0. One-and two-dimensional nuclear magnetic resonance (NMR) data suggest that purified p16 from our construct has a unique folded conformation under our experimental conditions and exhibits quite stable conformational characteristics.

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Isolation of Biologically Active Compounds from the Flower Petals of Carthamus tinctorius L. (홍화(Carthamus tinctorius L.)로부터 활성물질의 분리)

  • Kim, Yung-Hee;Ahn, Eun-Mi;Bang, Myun-Ho;Nam, Ji-Youn;Kwon, Byung-Mok;Baek, Nam-In
    • Applied Biological Chemistry
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    • v.41 no.2
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    • pp.197-200
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    • 1998
  • The MeOH extracts obtained from the flower petals of Carthamus tinctorius were solvent-fractionated with EtOAc, n-BuOH, and $H_2O$, successively. From the n-BuOH extract 2 flavonoid compounds were isolated through the repeated silica gel column chromatographies. From not only the results of physico-chemical data including HMBC but also the adaptation of acid hydrolysis, the chemical structures of the compounds were determined as $3-O-[{\beta}-D-glucopyranosyl(1{\rightarrow}2)\;{\beta}-D-glucopyranosyl]\;kaempferol$ and $3-O-[{\alpha}-L-rhamnopyranosyl(1{\rightarrow}6)\;{\beta}-D-glucopyranosyl]\;kaempferol$. The compounds exhibited $IC_{50}$ values in Grab2-Shc activity to be 43 and $47{\mu}g/ml$, respectively.

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Synthesis and Properties of Hyperbranched Liquid Crystalline Polyesters by Direct Polycondensation (직접중축합법에 의한 하이퍼브랜치 액정 폴리에스터의 합성 및 성질)

  • Park, Jong-Ryul;Kim, Hye-Mi;Yoon, Doo-Soo;Sohn, Jeong Sun;Bang, Moon-Soo
    • Applied Chemistry for Engineering
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    • v.28 no.2
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    • pp.237-244
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    • 2017
  • Hyperbranched liquid crystalline polymers with azomesogenic and cholesteryl groups in their terminal positions were designed and synthesized by direct polycondensation reaction. The chemical structures and thermal and mesomorphic properties of the synthesized polymers were investigated by FT-IR, $^1H-NMR$, differential scanning calorimetry (DSC), thermogravimetry analysis (TGA), and polarizing optical microscopy (POM). The inherent viscosities (${\eta}_{inh}$) of the polymers were measured to be between 0.30 and 0.50 dL/g in phenol/p-chlorophenol/1,1,2,2-tetrachloroethane (25/40/35 = w/w/w). The degree of branching (DB) in these polymers ranged from 0.37 to 0.75; they, as amorphous polymer, showed glass transition temperatures ranging from 80 to $120^{\circ}C$; the polymers readily dissolved in most of the organic solvents used in the experiments. Only hyperbranched polymers with a cholesteryl group as their mesogenic group showed liquid crystalline phases.

Preparation and Properties of Aromatic Polybenzoxazoles with high char yields (높은 char 수득률를 갖는 방향족 polybenzoxazoles의 제조 및 특성)

  • Sohn, Jun-Youn;Moon, Sung-Chul;Yoon, Doo-Soo;Choi, Jae-Kon
    • Elastomers and Composites
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    • v.42 no.4
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    • pp.238-248
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    • 2007
  • A series of polyhydroxyamides(PHAs) having ether linkages in the polymer backbone were prepared via solution polycondensation at low temperature. These polymers were studied by FT-IR, $^1H-NMR$, DSC, TGA and PCFC. The PHAs exhibited inherent viscosities in the range of $0.5{\sim}1.1dL/g\;at\;35^{\circ}C$ in DMAc solution. Most of PHAs except PHA 3 were soluble in polar organic solvents such as N,N-dimethylacetamide(DMAc), N-methyl-2-pyrrolidone(NMP), and N,N-dimethylform-amide(DMF). Subsequent thermal treatment of PHAs afforded polybenzoxazols(PBOs). However, the PBOs were insoluble in a variety of solvents. Most of the PBOs except PBO 3 showed glass-transition temperature($T_g$) in the range of $200{\sim}246^{\circ}C$ by DSC and maximum weight loss temperature in the range of $597{\sim}697^{\circ}C$ in nitrogen by TGA. PBOs showed high char yields in the range of $51{\sim}64%$. PCFC results of the PBOs showed the heat release(HR) capacity, $8{\sim}65J/gK$ and total heat release(total HR), $2.4{\sim}4.7kJ/g$.

Optimization of D-\beta-hydroxybutyric Acid Fermentation Using a Mutant of Candida Rugosa IFO0750 (Candida rugosa 변아주를 이용한 D-\beta-Hydroxybutyric Acid 발효공정의 최적화)

  • 경수현;신철수
    • Microbiology and Biotechnology Letters
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    • v.28 no.6
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    • pp.355-360
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    • 2000
  • A UVmutant of Candida rugosa IF00750 was made and used to convert butYlic acid to D-$\beta$-hydroxybutyric acid(D-$\beta$-HBA). Major regulating factors for D-$\beta$-HBA fennentation were investigated via chemostat analyses. The maximum specific productivity was achieved at a specific growth rate of $0.06h^{-1}$ where the glucose and butyric acid concentrations in the fermentor were 10 g/L and 8.7 g/L. respectively. A fed-batch fennentation was performed with maintenance of the optimum glucose and butyric acid concentrations. The D-$\beta$-HBA concentration after 120 h of cultivation reached 12.4 g/L, which was 4.7 times greater illan the concentration obtained by batch fermentation.

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