• Title/Summary/Keyword: $^2H$ NMR

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버들송이로부터 분리한 Nucleoside계 화합물의 지질과산화 저해활성 (A Nucleoside with Lipid Peroxidation Inhibitory Activity from Agrocybe cylindracea.)

  • 이인경;윤봉식;유익동
    • 한국미생물·생명공학회지
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    • 제26권6호
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    • pp.558-561
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    • 1998
  • 식용버섯인 버들송이(Agrocybe cylindracea)로부터 새로운 생리활성물질을 탐색하던 중 버들송이 자실체의 methanol 추출물로부터 Diaion HP-20 column chromatography, ethyl acetate extraction 및 silica gel column chromatography를 행하여 AG 8을 분리하였다. 분리된 AG 8의 구조해석을 위하여 Mass, $^1$H 및 $^{13}$C NMR, irradiation실험 및 HMBC를 실시한 결과 분자량이 297, 분자식이 $C_{11}$ $H_{15}$$N_{5}$$O_3$S인 nucleoside계 화합물 5'-deoxy-5'-methylthioadenosine(MTA)으로 동정하였다. AG 8의 지질과산화 저해활성은 $IC_{50}$/ 값이 3.2 $\mu\textrm{g}$/$m\ell$ 이었으며 양성 대조구인 vitamin E보다 3배 정도 낮은 활성을 보여주었다. 본 화합물은 고등동물의 대사과정에 관여하는 효소 대사 조절물질로 고등동물을 비롯한 각종 생물체에 존재하는 것이 보고되었으나 담자균류로부터는 본 연구에 의하여 처음 분리되었다.

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Deuterium Naturally Present in Solvent and Site-Specific Isotope Population of Deuterium-Enriched Solute

  • Hwang, Ryeo Yun;Han, Oc Hee;Lee, Juhee;Kim, Eun Hee
    • Bulletin of the Korean Chemical Society
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    • 제34권10호
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    • pp.2959-2962
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    • 2013
  • As the concentration of aqueous $CD_3OH$ solutions was decreased, the OD peaks in $^2H$ NMR spectra grew relative to the $CD_3$ peaks. Isotope impurity for OH groups of $CD_3OH$ and deuterium naturally present in water contributed to the OD peaks. Using these peak area data, the site-specific isotope populations of isotope enriched chemicals were measured. In addition, the method using both $^1H$ and $^2H$ NMR spectroscopy was demonstrated with neat $CD_3OH$ to measure the site-specific isotope populations. The results indicate that although it represents only ~0.015% of hydrogen isotopes, the deuterium naturally present in solvents cannot be ignored, especially when the concentration of deuterium-enriched solutes is varied. Proton/deuteron exchange between methyl and methyl/hydroxyl groups was confirmed to be negligible, while that among hydroxyl groups was detectable.

단삼(丹蔘)으로부터 항균물질의 분리 (Isolation of Antimicrobial Compounds from Salvia miltiorrhiza Bunge)

  • 한완수
    • 한국약용작물학회지
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    • 제12권3호
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    • pp.179-182
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    • 2004
  • 단삼(丹蔘)을 bioassay-directed fractionation에 의한 에탄올 추출물의 클로로포롬 분획물을 silica gel column chromatography, recycling preparative-HPLC 등을 실시하여 항균활성을 나타내는 2개의 화합물을 분리하여 이화학적 성상 및 spectra data (IR,$^1H-NMR,\;^{13}C-NMR$ 및 Mass)에 의해 각각 Cryptotanshinone과 dihydrotanshinone I으로 동정하였으며, 이들 화합물의 항균성 (MIC)은 각각 S. epidermidis에 대하며 $6.3,\;3.1\;{\mu}g/ml$와 S. pyogenes에 대해 $6.3\;{\mu}g/ml$로 비교적 높은 활성을 나타내어 항생제로서 개발 가능성을 보여주었다.

An NMR Study on Complexation of Ethylammonium Ion by Alkyl p-tert-Butylcalix[6]aryl Ester Derivatives

  • 안상두;문철순;정기주;이조웅;오원석;장석규
    • Bulletin of the Korean Chemical Society
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    • 제19권1호
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    • pp.68-74
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    • 1998
  • The complexation of ethylammonium ion by alkyl p-tert-butylcalix[6]aryl ester derivatives was studied via measurements of proton and carbon spin-lattice relaxation times $(T_1)$ and chemical shift changes in solution state $(CDCl_3)$. The results indicate that the endo-type complexes are formed and that the overall tumbling rates of these complexes are more rapid than those of the corresponding free hosts. The association constants for these complexes in $THF-d_8$ were determined by $^1H$ NMR titration at several different temperatures to estimate the relevant thermodynamic parameters. The logK's for ethylammonium complexes of methyl, ethyl, and propyl esters at 313 K, for example, were found to be 1.56, 3.41, and 3.08, respectively. The complexes formed may be thought of as being kinetically stable in view of their $^1H$ NMR behavior in 2 : 1 host/guest solution.

$^{207}Pb-NMR$ 분광법에 의한 $Pb(II)-N_2O_m$계 거대고리 리간드 착물형성 반응의 교환 메카니즘 (Exchange Reaction Mechanism of $Pb(II)-N_2O_m$ Macrocyclic Complexes by $^{207}Pb-NMR$ Spectroscopy)

  • 김정;윤창주;유한준;김건;김시중
    • 대한화학회지
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    • 제38권1호
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    • pp.41-49
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    • 1994
  • Pb(II)이온과 질소-산소 주개 거대고리 리간드인 1,13-diaza-3,4 : $1011-dibenzo-59-dioxacyclohexa-decane(NtnOtnH_4)$, 1,15-diaza-3,4 : $1213-dibenzo-5811-trioxacycloheptadecane(NenOdienH_4)$, 및 1,15-diaza-3,4 : $1213-dibenzo-5811-trioxacyclooctadecane(NtnOdienH_4)$간의, 착물 형성 반응에서 Pb(II)이온에 대한 교환 반응 메카니즘을 $^{207}Pb-NMR$분광법을 사용하여 N,N'-dimethylformamide(DMF)용액에서 조사하였다. $Pb(II)-NtnOtnH_4$계에서는 주로 회합-해리 메카니즘에 의해 교환 반응이 진행되고 있었으며 $Pb(II)-NtnOdienH_4계$의 경우, $-5^{\circ}C$ 이하의 온도 영역에서는 이분자 교환 메카니즘으로, $+5^{\circ}C$ 이상의 온도영역에서는 회합-해리 메카니즘과 이분자 교환 메카니즘이 동시에 교환 반응에 영향을 미치고 있다. 또한 해리 반응에 대한 활성화 에너지는 $NtnOdienH_4\;<\;NtnOtnH_4\;<\;NenOdienH_4$의 순으로 착물의 안정도 상수와는 반대의 순이었다.

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분광계에 의한 Borosilicate계 글라스의 조성 및 온도의존성 평가 (Composition and Temperature Dependence of Structural Changes in Borosilicate Glasses by Spectrometer)

  • 박성제;류봉기
    • 한국재료학회지
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    • 제15권12호
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    • pp.786-790
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    • 2005
  • We investigated the particularity of temperature and composition changes in $xNa_2O{\cdot}(52.5-x)B_2O_3{\cdot}47.5SiO_2$ glasses by use of FT-IR, $^{11}B$ NMR, Raman spectrometer. From FT-IR and $^{11}B$ NMR spectrometer, we thought that tetrahedral boron, $BO_4$ units are created $N_4$ increasing tendency generated near $600^{\circ}C$. It's expected that composition ana heat treatment directly contributed to structural changes, this changes are following to $Na_2O$ increasing or decreasing. caused by $N_4\;and\;BO_4$ units are caused by relatively increasing or decreasing in the glasses' structure. Particularly, $BO_4$ units are converted to $BO_3$ units after $600^{\circ}C$ heat treatment for 50h in the composition of $x<18(R<0.5,\;R=Na_2O/B_2O_3\;mol\%)$. On the order hand, $BO_3$ units are converted to, $BO_4$ units after $600^{\circ}C$ heat treatment for 50h in the composition of $x{\geq}18\;(R>0.5)$. This particularity of composition and temperature dependence of structural changes are similarly represented by Raman analysis results.

Bacillus subtilis JW-1 균주가 생산하는 bacilysin의 풋마름병 억제 효과 및 특성 (Isolation and characterization of bacilysin against Ralstonia solanacearum from Bacillus subtilis JW-1)

  • 김신덕
    • 미생물학회지
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    • 제54권2호
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    • pp.136-139
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    • 2018
  • 풋마름병 균에 대해 강한 저해활성을 갖는 활성물질 Compound S와 conversion product인 compound S'이 Bacillus subtilis JW-1 배양액에서 일련의 크로마토그래피 방법으로 분리 정제되었고, $^1H$ NMR, $^{13}C$ NMR, $^1H-^1H$ COSY와 HMBC 등의 spectra 분석에 의해 구조가 alanyl-L-${\beta}$-(2,3-epoxycyclohexyl-4-one)alanine와 alanyl-L-${\beta}$-(2,3-dihydroxycyclohexyl-4-one) alanine로 각각 동정되었다. Compound S는 $G^+$, $G^-$ bacteria, yeast와 Candida albicans 등에 대해 광범위한 antimicrobial activity를 나타내며, conversion product의 활성 상실을 통해 intact oxirane ring이 Compound S의 활성에 필수적임이 밝혀졌다.

Purification and Properties of Non-Cariogenicity Sugar Produced by Alkalophilic Bacillus sp. S-1013

  • Ryu, Il-Hwan;Kim, Sun-Sook;Lee, Kap-Sang
    • Journal of Microbiology and Biotechnology
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    • 제14권4호
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    • pp.751-758
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    • 2004
  • The NCS(Non-Cariogenicity Sugar) from Bacillus sp. S-1013 was purified by cold acetone and methanol precipitation, and DEAE-cellulose ion-exchange and Sephadex G-100 column chromatographies, to yield an amorphous yellow syrup. The melting point and $[\alpha]_D^{20}$ were 155-$157^{\circ}C$ and +53, respectively. Instrumental analyses such as FT-IR, $^1H-NMR, and ^{13}C-NMR$ showed that the NCS contained an O-H group, C-H, C=O, $NH_2$, anomeric carbon, anomeric proton, N-acetylgalactose, fucose, and neuramic acid, thus, the NCS was determined to be a trisaccharide of Fuc($1\longrightarrow4$)GalNAc($2\longrightarrow6$) NeuAc.

Preparation and Characterization of Dinuclear Metal Complexes, $[(PPh_3)_2(CO)M({\mu}-E)M(CO)(PPh_3)_2](SO_3CF_3)_2$ (M = Rh, Ir; E = 1,4-Dicyanobenzene and 1,4-Dicyano-2-butene)

  • Moonsik Kim;JaeKyun Chin;Jaejung Ko
    • Bulletin of the Korean Chemical Society
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    • 제13권5호
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    • pp.556-559
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    • 1992
  • Hydrocarbon solution of $(PPh_3)_2(CO)MOSO_2CF_3$ (M= Rh, Ir) reacts rapidly with 1,4-dicyanobenzene or 1,4-dicyano-2-butene to yield dinuclear metal complexes $[(PPh_3)_2(CO)M({\mu}-dicyanobenzene)M(CO)(PPh_3)_2](SO_3CF_3)_2$ (I: M = Rh; II: M = Ir) or $[(PPh_3)_2(CO)M({\mu}-dicyano-2-benzene)M(CO)(PPh_3)_2](SO_3CF_3)_2$ (III: M = Rh; IV: M = Ir), respectively. Compounds I, II, III, and IV were characterized by $^1H$-NMR, $^{31}P$-NMR, and infrared spectrum. Dichloromethane solution of II and IV reacts with $H_2\;and\;I_2$ to yield oxidative addition complexes $[(PPh_3)_2(CO)IrX_2({\mu}-E)X_2Ir(CO)(PPh_3)_2](SO_3CF_3)_2$ (V; E = 1,4-dicyanobenzene, $X_2$ = $H_2$; VI : E = 1,4-dicyano-2-butene, $X_2$ = $H_2$; VII; E = 1,4-dicyanobenzene, $X_2$ = $I_2$). All metal complexes are bridged by the cyanide groups. Compounds Ⅴ, Ⅵ, and Ⅶ are characterized by conventional methods.

NMR Studies of Ni-binding Luteinizing Hormone Releasing Hormone

  • Kim, Jin;Won, Ho-Shik
    • 한국자기공명학회논문지
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    • 제13권2호
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    • pp.143-153
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    • 2009
  • Luteinizing Hormone Releasing Hormone (LHRH) is composed of 10 amino acids, and is best known as a neurotransmitter. Because of the 80% homology in animals, much more concerns have focused on the substances that have similar functions or can control LHRH. Ni, Cu-LHRH complexes were synthesized. The degree of complexation was monitored by $^1H,\;^{13}C$-NMR chemical shifts, and final products were identified by ESI-Mass spectrum. Solution-state structure determination of Ni-LHRH complex was accomplished by using NMR results and NMR-based distance geometry (DG). Interproton distances from nuclear Overhauser effect spectroscopy (NOESY) were utilized for the molecular structure determination. Results were compared with previous structures obtained from energy minimization and other spectroscopic methods. Structure obtained in this study has a cyclic conformation which is similar to that of energy minimized, and exhibits a specific a-helical turn with residue numbers (2~7) out of 10 amino acids. Comparison of chemical shifts and EPR studies of Ni, Cu-LHRH complexes exhibit that Ni-LHRH complex has same binding sites with the 4-coordination mode as in Zn-LHRH complex.