• Title/Summary/Keyword: $^1H-NMR$ Spectrum

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Assignment of the Redox Potentials of Cytochrome c₃of Desulfovibrio vulgaris Hildenborough by ¹H NMR

  • 박장수;강신원;신정휴
    • Bulletin of the Korean Chemical Society
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    • v.16 no.10
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    • pp.968-971
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    • 1995
  • The heme assignment of the 1H NMR spectrum of cytochrome c3 of Desulfovibrio vulgaris Hildenborough within the X-ray structure were fully cross established according to their redox potential. The major reduction of the heme turned out to take place in the order of hemes Ⅳ,Ⅰ,Ⅱ and Ⅲ(the heme numbers indicating the order of bonding to the primary sequence). This assignment can provide the physicochemical basis for the elucidation of electron transfer of this protein.

Purification and Chemical Characterization of Antibiotic MT-497 Produced by Streptomyces nigrifaciens GMT-497 (Streptomyces nigrifaciens GMT-4967이 생산하는 항생물질 MT-497의 분리와 화학적 특성)

  • 이영선;안순철;윤병대;민태익;이정형;이현선;안종석;민태익
    • Microbiology and Biotechnology Letters
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    • v.19 no.6
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    • pp.604-609
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    • 1991
  • Antibiotic MT-497 was purified from the culture broth of Streptomyces nigr$^1H-NMR$ and composition of amino acids, MT-497 was identified as one of the actinornycin antibiotics containing actinocin chromophore and the peptide with threonine, proline, methyl valine, sarcosine and aspartic acid.

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$^1H$ NMR Study of 4-Aminopyrimidine Coordinated to the Paramagnetic Undecatung-stocobalto(Ⅱ)silicate Anion: Rates of Internal Rotation of the Amine Group

  • 김병안;소현수
    • Bulletin of the Korean Chemical Society
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    • v.20 no.10
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    • pp.1149-1152
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    • 1999
  • 1H NMR spectrum of a DMF-d7 solution containing 4-aminopyrimidine and [SiW11CoIIO39]6- (SiW11Co) shows separate peaks from two linkage isomers, a and b, in which N(1) and N(3) of the pyrimidine ring are coordinated to SiW11Co, respectively. The signal from the amine group in the isomer a exhibits temperature dependence that is characteristic of a two-site exchange problem. Rates of internal rotation of the amine group were determined by simulating the NMR spectra at 5-35℃. The amine group of free 4-aminopyrimidine also shows temperature-dependent spectra at lower temperatures; rates of internal rotation at (-25)-25℃ were determined. The internal rotation of the amine group in the complex is much slower than that for free 4-aminopyrimidine, indicating that π-character of the C-N bond increases on coordination to SiW11Co. The amine group in the isomer b does not show such behavior. It is probable that hydrogen bonding between N-H and a bridging oxygen atom of SiW11Co prevents it from rotating at low temperatures.

Synthesis and Characterization of Palladium (IV) Complexes with Guanine, Adenine, and Uracil Base (Guanine, Adenine 및 Uracil 염기를 갖는 팔라듐 (IV) 착물의 합성과 그 성질)

  • Oh Sang Oh;Chung Duck Young;Kim Hee Seon
    • Journal of the Korean Chemical Society
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    • v.36 no.5
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    • pp.679-684
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    • 1992
  • New Pd(IV) complexes have been prepared through the reactions of $trans-[Pd(en)_2Cl_2](ClO_4)_2 $(en = ethylenediamine) with Guanine, Adenine, or Uracil anion as purine and pyrimidine base. We identified the ratio of central metal versus ligands by $C{\cdot}H{\cdot}N$ elemental analysis and proposed the coordinating site of the base by infrared spectrum, $^1H-NMR,\; and\; ^{13}C$-NMR spectrum. Guanine or Adenine ligand coordinated at N7 site and an en ligand exchanged for $ClO_4^-$ counter ions of the starting material . As these results, the complexes showed the formula $[Pd(en)L_2(ClO_4)_2](ClO_4)_2{\cdot}(en)$, (L = Guanine, Adenine). But in the Uracil complex no exchange of the en ligand and $ClO_4^-$ occured and Uracil anion preferred the N1 to N3 as coordinating site, the complex $[Pd(en)_2(Urac)_2](ClO_4)_2(Urac = Uracil anion).$

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Isolation and Identification of Antimicrobial Compound from Amarantus lividus (참비름 추출물에서 항균성 물질의 분리 및 동정)

  • Oh, Young-Sook;Lee, Shin-Ho
    • Microbiology and Biotechnology Letters
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    • v.33 no.2
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    • pp.123-129
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    • 2005
  • Isolation and identification of pathogens from slaughter and meat processing plant were investigated. Antimicrobial activity of Amaranthus lividus against isolated pathogens such as Aeromonas sobria, Escherichia coli, Escherichia coli O157, Listeria monocytogenes, Salmonella spp., and Staphylococcus aureus was investigated. Among the chloroform, ethyl acetate and buthanol fraction of amaranthus lividus showed inhibitory effect against Aeromonas sobria CLFM1 and Escherichia coli CLFM2. Antimicrobial substance in chloroform fraction was isolated by silica gel adsorption column chromatography, sephadex LH-20 column chromatography and silica gel partition column chromatography. The antimicrobial compound of amaranthus lividus was identified as diethyl phtalate by HPLC, GC-MS, H-NMR and C-NMR.

Isolation and Purification of Berberine in Cortex Phellodendri by Centrifugal Partition Chromatography (Centrifugal Partition Chromatography에 의한 황백으로부터 Berberine의 분리 및 정제)

  • Kim, Jung-Bae;Bang, Byung-Ho
    • The Korean Journal of Food And Nutrition
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    • v.27 no.3
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    • pp.532-537
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    • 2014
  • Cortex Phellodendri (CP) is derived from the dried bark of Phellodendron amurense. It has been widely used as a drug in traditional Korea medicine for treating diarrhea, jaundice, swelling pains in the knees and feet, urinary tract infections, and infections of the body surface. Many analytical methods have been used to study oriental herbal medicines, such as thin-layer chromatography, column liquid chromatography, and high performance liquid chromatography (HPLC). In this study, preparative centrifugal partition chromatography (CPC) was successfully carried out in order to separate pure compounds from a CP methanol extract. The optimum two-phase CPC solvent system was composed of n-butanol: acetic acid: water (4:1:5 v/v/v). The flow rate of the mobile phase was 3 mL/min in ascending mode with rotation at 1,000 rpm. The CPC-separated fraction and purification procedures were carried out by preparatory HPLC. The $^1H$ NMR spectrum revealed that the resonances at ${\delta}$ 4.10 and 4.20 ppm corresponded to three protons ($-OCH_3$), whereas those at ${\delta}$ 6.10 ppm corresponded to two protons ($-OCH_2O-$). Further, two aromatic protons (H-11 and H-12) conveys a doublet-doublet pattern. The H-11 doublet and H-12 doublet appear at ${\delta}$ 7.98 and 8.11, respectively. The $^{13}C$ NMR. spectrum showed a tetrasubstituted with a methylenedioxy group at C2 and C3, and two methoxy groups at C9 and C10. The chemical structure of the berberine was identified by $^1H$, $^{13}C$-nuclear magnetic resonance and electrospray ionization-mass spectroscopy spectral data analysis.

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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Structural Analysis of Natural Indigo Colorants Extracted from polygonum tintorium (쪽풀에서 추출한 천연 인디고 색소의 구조 분석)

  • 정인모;김인회;남성우
    • Textile Coloration and Finishing
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    • v.10 no.3
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    • pp.20-28
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    • 1998
  • Natural indigo colorants were prepared by extraction of polygonum tintorium which was harvested just in the blooming season(in the late of July). The components were analyzed by TLC and HPLC, and its structures were analyzed by FT-IR, EI-mass and NMR. The dyeing mechanism and fermentation conditions were investigated. Its colour fastness was studied as well. The results obtained are summarized as follows ; The natural indigo powder was dissolved in DMSO and developed in eluent, $CHCl_3/CH_3CN(8.5:1.5v/v)$ by means of TLC for its quality analysis. It was segregated into indirubin as il red colour and indigo as a blue colour. In case of HPLC analysis, the retention times of indirubin and indigo were 7.442 and 6.543, respectively. FT-IR spectrum of indirubin showed a peak for NH residue between 3200 and $3300cm^{-1}.^1H-NMR$ spectrum for indigo displayed AA'BB' spin system caused by indole structure between 6.5 and 7.7ppm of H4, 5, 6 and 7, and -NH proton for indirubin showed an singlet between 10.88 and. 11.0ppm. EI-mass spectrum of indigo an d indirubin both disclosed their molecular size as 262 and it implies that these two substances are isomer.

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Quantitative Analysis of Coumarins from Angelica gigas Using $^1H$-NMR

  • Yoo, Jong-Su;Ahn, Eun-Mi;Song, Myoung-Chong;Bang, Myun-Ho;Kim, Dong-Hyun;Han, Min-Woo;Kwak, Ho-Young;Lee, Dae-Young;Lyu, Ha-Na;Baek, Nam-In
    • Food Science and Biotechnology
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    • v.17 no.3
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    • pp.573-577
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    • 2008
  • $^1H$-Nuclear magnetic resonance (NMR) spectrometry was applied to the quantitative analysis of coumarins in the roots of Angelica gigas without any chromatographic purification. The experiment was performed by the analysis of each singlet germinal methyl, which was well separated in the range of 1.0-2.0 ppm in the $^1H$-NMR spectrum. The quantity of the compounds was calculated by the ratio of the intensity of each compound to the known amount of internal standard (dimethyl terephthalate). These results were compared with the conventional gas chromatography (GC) method. The contents of decursin and decursinol angelate in A. gigas were determined $1.98{\pm}0.07$, $1.13{\pm}0.08%$ in quantitative $^1H$-NMR method and $2.06{\pm}0.24$, $1.17{\pm}0.24%$ in GC method, respectively. The advantages of quantitative $^1H$-NMR analysis are that can be analyzed to identify and quantify, and no reference compounds required for calibration curves. Besides, it allows rapid and simple quantification for coumarins with an analysis time for only 10 min without any preprocessing.

Synthesis of Multisubstrate analog Inhibitor of Thymidylate synthase (Thymidylate Synthesis의 Multisubstrate analog Inhibitor의 합성)

  • Kwak, In-Young;Ryu, Eung-K
    • The Journal of Natural Sciences
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    • v.4
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    • pp.23-28
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    • 1991
  • The pyrimidy1 derivative of 2'-deoxythmidine 5'-monophosphate, 3 has been synthesized for the development of anticanncer agents. The compound 3 derived from prototype inhibitor 2 by modifying the p-aminobenzoy1 glutamic acid portion has been designed to facilitate the membrane penetration. Variable temperature $^1H$ NMR spectrum for the protected nucleotide has indicated the existence of two conformers which are stable on the NMR time scale at ambient temperature.

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