• 제목/요약/키워드: 1H-NMR spectroscopy

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1H-NMR 스펙트럼의 다변량통계분석을 통한 넙치(Paralichthys olivaceus)의 백신 반응의 지표물질 분석 (Multivariate Analysis on 1H-NMR Spectroscopy of Olive Flounder Paralichthys olivaceus Serum)

  • 조지영
    • 한국수산과학회지
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    • 제45권4호
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    • pp.367-371
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    • 2012
  • To investigate the relationship between metabolic changes in $^1H$-nuclear magnetic resonance (NMR) spectra and fish vaccination, serum was collected from olive flounders treated with a formalin-killed Edwardsiella tarda vaccine and used for $^1H$-NMR metabolite profiling. Principal component analysis and partial least squares were applied to the $^1H$-NMR profile to reduce its complexity and establish class-related clusters. Relative lipid regions were distinguished in vaccinated and non-vaccinated serum. Then, the lipids were extracted from the serum and analyzed. Triolein was identified.

대장균 베타-갈락토시데이즈를 이용하여 합성된 1, 2-Hexanediol Galactoside의 NMR Spectroscopy 및 Mass spectrometry (NMR Spectroscopy and Mass Spectrometry of 1, 2-Hexanediol Galactoside synthesized using Escherichia coli β-Galactosidase)

  • 김이옥;이향렬;정경환
    • 한국응용과학기술학회지
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    • 제33권2호
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    • pp.286-292
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    • 2016
  • 화장품용 방부제로 사용하고 있는 1, 2-hexanediol (HD)에 높은 농도의 lactose (300 g/l)를 넣고, 재조합 대장균 ${\beta}$-galactosidase (${\beta}$-gal)를 이용하여 galactose 한 분자를 결합시키는 transgalactosylation 반응을 시켜서, 1, 2-hexanediol galactoside (HD-gal)을 합성하였다. 그리고, 합성된 HD-gal 분자를 확인하기 위하여, HD-gal에 대한 NMR ($^1H$- and $^{13}C$-) 스펙트럼 분석과 mass 스펙트럼 분석을 실시하였다. HD-gal의 $^1H$ NMR 스펙트럼에서 HD에 갈락토실화가 되었음을 보여주는 다양한 피크를 확인하였다. $^1H$ NMR 스펙트럼의 다운필드인 ${\delta}_H$ 4.44 ppm과 ${\delta}_H$ 3.96~3.58 ppm에서 나타나는 다양한 피크들은 HD에 갈락토실화가 되었다는 것을 잘 암시하고 있으며, 또한 $^1H$ NMR 스펙트럼의 업필드에서 나타나는 ${\delta}_H$ 1.60~1.35 ppm과 0.92 ppm의 피크는 HD의 $CH_2$$CH_3$ 작용기로부터 나타나는 피크로써 HD가 본 물질에 존재한다는 것을 나타내고 있다. $^{13}C$ NMR 스펙트럼에서는 HD-gal의 알파-아노머와 베타-아노머의 구조에서 기인하는 총 21의 카본피크가 나타났고, 각 아노머마다 12개의 카본이 존재하는데 이중 ${\delta}_C$ 68.6, 60.9 and 13.2 ppm에 보이는 3개의 카본은 겹쳐서 나타나 총 24개의 피크 중 21개가 나타났다. 또한, 질량스펙트럼 분석에서는 protonated HD-gal인 281.1601 (m/z)의 peak를 확인할 수 있었다. 이를 종합하면, NMR ($^1H$- and $^{13}C$-) 스펙트럼 분석 결과와 질량분석 결과들은 우리가 기대했던 HD-gal의 구조와 매우 잘 일치하고 있다는 것을 알 수 있었다. 앞으로 추가적으로, 세균에 대한 minimum inhibitory concentrations (MICs) 조사와 human skin cell에 대한 독성연구를 추가적으로 진행할 예정이며, 이러한 결과를 근거로 항균력을 유지하면서 피부세포에 대한 독성이 감소된 화장품용 방부제의 연구/개발이 계속되기를 기대하고 있다.

해면 Luffariella sp.의 화학적 성분 연구 (A Study on the Chemical Constituents from Marine Sponge Luffariella sp.)

  • 박선구;김성수;박준대;홍정선;김인규
    • 대한화학회지
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    • 제39권7호
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    • pp.559-563
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    • 1995
  • 인도네시아 Manado만의 Sulawesi에서 채집한 KB cancer cell line에 대해 in vitro로 활성을 갖는 해면 Luffariella sp.으로부터 Germacrene alcohol(1), Aaptamine(2) 및 Hexacyclic terpene(3)을 분리하였으며, 1에대한 spectral data는 문헌치와 비교${\cdot}$분석하여 수정하였다. 이들을 $^1H$, $^13C$ NMR, $^1H$ $^13C$(bond) Heteronuclear Multiple Quantum Coherence Spectroscopy(HMQC), $^1H$$^13C$(2 and 3 bond)Heteronuclear Multiple Bond Correlation Spectroscopy(HMBC), Electron Impact Mass Spectroscopy(EI ms), UV 및 IR에 의해 밝혔다.

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Influence of Hot Pressing on the Pore Structure of Nafion Electrolyte Membrane Investigated by 1H NMR

  • Jeonga, Soon-Yong;Han, Oc-Hee
    • Bulletin of the Korean Chemical Society
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    • 제30권7호
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    • pp.1559-1562
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    • 2009
  • The influence of hot pressing on the pore structures of Nafion membranes was investigated by observing the Nafion before and after hot pressing with $^1H$ nuclear magnetic resonance (NMR) spectroscopy. The freezing point depression and chemical shift data of water in the Nafion indicated the presence of two different pore size ranges in Nafion. Hot pressing mainly reduced the sizes and number of the big pores. The reduction of water uptake and proton conductivity after hot pressing was explained by this variation of pore size and number. We demonstrated the potential application of chemical shift data and NMR cryoporometry experiments to measure the relative pore sizes, on a nano scale, and numbers.

Trichoderma koningii에서 분리한 저분자 1, 4-$\beta$-D-Glucan Glucanohydrolase의 반응산물에 대한 핵자기공명 스펙트럼 분석 ($^{1}H-NMR$ Spectroscopic Evidence on the Glycosidic Linkages of the Transglycosylated Products of Low-Molecular-weight 1,4-$\beta$-D-Glucan Glucanohydrolase from Trichoderma koningii)

  • 맹필재;강사욱;정춘수;홍순우;하영칠;이영하;김재헌
    • 미생물학회지
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    • 제25권4호
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    • pp.304-308
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    • 1987
  • The mode of transglycosylation reaction observed during the action of low-molecular-weight 1,4-$\beta$-D-glucan glucanohydrolase (EC 3.2.1.4) purified from Trichoderma koningii ATCC 26113 was investigated using $^{1}H-NMR $spectroscopy. The H-1 proton resonances were analysed. After reaction of the enzyme with cellotriose, the reaction products were separated by high performance liquid chromatography. H-1 resonances of the products were consisted with those of cellobiose, cellotriose and cellotitraose, respectively. Therefore it was proved that all the reaction products formed by the action of the enzyme on cellooligosaccharides, including transglycosylation products, possess only H-NMR -1,4-glycosidic linkage(s).

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다양한 치환기가 붙은 Styryl 4-Methoxy-1-Naphthyl Ketone의 합성과 치환기 효과에 관한 연구 (Synthesis and Substituent Effects in Substituted Styryl 4-Methoxy-1-Naphthyl Ketones)

  • Thirunarayanan, G.;Ananthakrishna Nadar, P.
    • 대한화학회지
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    • 제50권3호
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    • pp.183-189
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    • 2006
  • 초음파를 이용한 응축 반응을 이용하여 다양한 치환기가 붙은 4-methoxy-1-naphthyl ketone화합물들을 90% 이상의 높은 수율로 합성하였으며, 생성된 화합물물들을 미세 분석법, IR, 1H, 13C NMR 분석법 등을 이용하여 확인하였다. IR 스펙트럼에서 s-cis와 s-trans C=O stretching 모드를 확인하였으며, NMR 데이터로부터 에틸렌의 탄소와 수소에 대한 chemical shift를 확인하였다. 이러한 분광데이터를 이용하여 여러 분자들에 대한 Hammet 치환기 상수 값 들을 얻을 수 있었으며, 이들로부터 가용매 분해반응에 미치는 치환기 효과를 해석할 수 있었다.

pH 변화에 따른 Tungstophosphates 화합물의 분자형태 변화에 대한 분광학적 연구 (A Study on the Molecular Changes of Tungstophosphate Species at Different pH Values using Spectroscopy)

  • 안범수
    • 한국응용과학기술학회지
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    • 제28권3호
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    • pp.284-289
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    • 2011
  • All spectroscopic methods used in this work indicate the instability of tungstophosphates in aqueous solutions and considerable dependence on pH with regard to the dominant species present in the solution. UV spectroscopy indicates that some changes occur in the system but they cannot be specified. IR spectroscopy gives more information on the identification of the dominant species as a function the pH of the solution. NMR spectroscopy provides unique data, which can be used for more accurate interpretation of changes in the solution of various pH values. In the case of aqueous solutions of tungstophosphates, the parent anion was present only in a very acidic solution of ca. pH 1. Some differences in interpretation of the molecular species present under various experimental conditions can be ascribed to some extent to the diversity of chemical shifts of NMR. Under physiological conditions attained with the addition of NaOH, tungstophosphates was dominantly present in the form of the lacunary monovacant anion.

Trichoderma koningii에서 분비되는 .$\beta$-D-glucosidase의 반응산물에 대한 핵자기공명분석 ($^{1}$H-NMR spectroscopic evidence on the glycosidic linkages of the transglycosylated products of low-molecular-weight $\beta$-D-glucosidase from trichoderma koningii)

  • 이헌주;정춘수;강사욱;하영칠
    • 미생물학회지
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    • 제27권1호
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    • pp.35-42
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    • 1989
  • The mode of transglycosylation reaction observed during the action of low-molecular-weigh $\beta$-D-glucosidase ($\beta$-D-glucoside glucohydrolase, EC3.2.1.21) purified from Trichoderma koningii ATCC 26113 was investigated using $^{1}H$-NMR spectroscopy. The enzyme was purified by the series of procedures including ammonium sulfate precipitation, and fractionations by column chromatographies on Bio-Gel P-150, DEAE-Sephadex A-50, and SP-Sephadex C-50. The final purification was performed by the band eluation after preparative polyacrylamide gel electrophoresis. The enzyme showed its molecular size of 78,000 through the analysis of sodium dodecyl sulfate-polyacrylamide gel electrophoresis and its isoelectric point of 5.80 through the analysis of analytical isoelectric focusing. The H-1 proton resonances were analyzed. After the reaction of the enzyme with cellobiose, the reaction products were separated by high performance liquid chromatography using refractive index detector. H-1 resonances of the products were consisted with those of gentiobiose [$\beta$-D-glucopyranosyl--(1,6)-D-glucopyranose], and cellotriose [$\beta$-D glucopyranosyl-(1,4)-$\beta$-D-glucopyranosyl]-(1,4)-D-glucopyranose] with minor resonances of sophorose [$\beta$-D-glucopyranosyl-(1,2)-D-glucopyranose], respectively.

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졸-겔법으로 합성한 TiO2-SiO2 분말의 분광학적 분석 (Spectroscopic Studies on the Preparation of Sol-Gel Derived TiO2-SiO2 Powder)

  • 정미원;염수진;이복임
    • 분석과학
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    • 제18권1호
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    • pp.1-4
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    • 2005
  • 반응 속도를 조절하기 위하여 유기 첨가제인 아세트산을 사용해 치환된 티타늄 이소프로폭사이드를 합성한 뒤 가수분해 시킨 실리콘(IV)에톡사이드와 반응시켜 $TiO_2-SiO_2$ 분말을 얻었다. 반응 과정 동안의 구조 변화와 특징을 NMR과 FT-IR을 통해서 살펴보았다. 열처리 과정을 거친 분말의 FT-IR 결과로부터 상 분리를 관찰하였다.

Isolation of Dineolignans, Saucernetin-7 and -8, with Nitric Oxide Inhibitory Activity and NMR assignment from Saururus chinensis

  • Lee, Kyung-Tae;Jung, Hyun-Ju;Park, Hee-Juhn
    • 한국자원식물학회지
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    • 제19권6호
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    • pp.655-659
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    • 2006
  • Two dineolignans (1,2) with nitric oxide inhibitory activities were isolated from Saururus chinensis (Saururaceae) using silica gel column chromatography. Although the structures, saucernetin-7 (1) and -8 (2), have been already reported, NMR assignment of the two compounds was completed aided by 2D-NMR spectroscopy including $^1H-^1H$ COSY, $^1H-^{13}C$ COSY, HMBC and NOESY NMR spectra. Compounds 1 and 2 exhibited significant nitride oxide inhibitory activity in LPS-induced RAW 264.7 cells with $IC_{50}$ values of $11.3{\mu}M\;and\;7.1{\mu}M$, respectively.