• Title/Summary/Keyword: 1D $^1H-NMR$

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Complete Assignment of $^{1}H$ and $^{13}C$-NMR Signals for (20S) and (20R)-Protopanaxadiol by 2D-NMR Techniques (2D-NMR 기법을 이용한 (20S)와 (20R)-Protopanaxadiol의 $^{1}H$- 및 $^{13}C$-NMR 완전 동정)

  • 백남인;김동선
    • Journal of Ginseng Research
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    • v.19 no.1
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    • pp.45-50
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    • 1995
  • (20S)- and (20R)-protopanaxadiol were prepared from crude ginseng saponin by chemical treatment. The $^{1}H$- and $^{13}C$-NMR signals of these compounds were fully assigned by various NMR techniques such as DEPT, 1H-1H COSY, HMQC, HMBC and NOESY.

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

  • 맹필재;강사욱;정춘수;홍순우;하영칠;이영하;김재헌
    • Korean Journal of Microbiology
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    • v.25 no.4
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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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Complete Assignment of $^1H-$ and $^{13}C-NMR$ Signals for (20S)- and (20R)-ginsenoside $Rh_2$ by 2D-NMR Techniques (2D-NMR 기법을 이용한 (20S)-와 (20R)-ginsenoside $Rh_2$$^1H-$$^{13}C-NMR$ Signals의 완전 동정)

  • Kim, Dong-Seon;Lee, You-Hui;Park, Jong-Dae;Jeong, So-Young;Lee, Chun-Bae;Kim, Shin-Il;Baek, Nam-In
    • Applied Biological Chemistry
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    • v.38 no.2
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    • pp.184-189
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    • 1995
  • (20S)- and (20R)-Ginsenoside $Rh_2$ were prepared from crude ginseng saponin by chemical treatments. The $^1H-$ and $^{13}C-NMR$ signals of these compounds were fully assigned by various NMR techniques such as DEPT, $^1H-^1H$ COSY, HMQC, HMBC and NOESY.

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Comparative analysis of glycerin in cosmetics by LC/MS and 1H NMR (LC/MS와 1H NMR을 이용한 화장품속의 글리세린 비교분석)

  • Park, Gyo-Beom;Park, Chan Jo;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.20 no.5
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    • pp.400-405
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    • 2007
  • The comparative analysis of glycerin in cosmetic samples was carried out by LC/MS and $^1H$ NMR spectrometry. For the LC/MS analysis, aqueous solution was controlled in strong basic condition with sodium hydroxide, and benzoyl chloride was added to the solution for the derivatization of glycerin. The derivative was extracted using pentane and analyzed by the LC/MS. For the $^1H$ NMR analysis, sample was directly dissolved in $D_2O$ solvent without pretreatment. The quantitative analysis of glycerin was done by $^1H$ NMR ERETIC method. The analysis results of LC/MS and $^1H$ NMR showed that the calibration curves were a good linearity with $r^2=0.9991$ in the range of 0.1 to $10{\mu}g/mL$ and $r^2=1$ in the range of 25 to $500{\mu}g/mL$, respectively.

Quantitative Analysis of Quality Control of Natural Medicine by $^1H-NMR$ Spectrometry-Quantitative Analysis of Hesperidin from Citrus unshiu ($^1H-NMR$을 이용한 한약재의 품질 평가 방법 확립;진피의 Hesperidin 정량분석)

  • Ahn, Eun-Mi;Baek, Mi-Young
    • The Korea Journal of Herbology
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    • v.23 no.3
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    • pp.27-32
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    • 2008
  • Objectives : In this paper, we describe that $^1H-NMR$ spectroscopy may be superior to the conventional HPLC for the quantitative analysis of hesperidin from Citrus unshiu. Methods : $^1H-NMR$ spectra (400 MHz) were recorded in $DMSO-d_6$ using a Varian UNITY Inova AS 400 FT NMR spectrometer. One hundred milligram of powdered Citrus unshiu was weighed out and mixed with 1 ml of $DMSO-d_6$ with sonication for 30 min (room temperature). The extracts were filtrated through a 0.45 ${\mu}m$ PVDF filter and 0.5 ml of filtrated extract used for quantitative $^1H-NMR$ measurement (added 1 mg of dimethyl terephthalate as internal standard). The quantity of hesperidin was calculated by the ratio of the intensity of the compound to the known amount of internal standard. For HPLC analysis, the half gram of plant material was extracted with 60 ml of MeOH for 2 hours. The extracts were made 100 ml volume and analyzed by a Waters HPLC system using a YMC ODS column. The total flow rate was 1.0 ml/min with a sample volume 10 ${\mu}l$ and UV detection at 280nm. Results : The contents of hesperidin in Citrus unshiu was determined $5.33{\pm}0.06$% in the quantitative $^1H-NMR$ method and $5.15{\pm}0.12%$ in HPLC method. Using the quantitative $^1H-NMR$ the contents of hesperidin can be determined in much shorter time than the conventional HPLC measurements. Conclusions : From those results, the advantages of quantitative $^1H-NMR$ analysis are that can be analyzed to identify and quantify, and no reference compounds required for calibration curve. Besides, it allows rapid and simple quantification for hesperidin with an analysis time for only 10 min without any pre-purification steps.

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Rates of Conformational Change of 3,3-Dimethylpiperidine and Solvent Effects on Its Conformation When Coordinated to the Paramagnetic Undecatungstocobalto(II)silicate Anion Studied by 1H NMR Spectroscopy

  • 현재원;소현수
    • Bulletin of the Korean Chemical Society
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    • v.18 no.9
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    • pp.961-965
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    • 1997
  • 1H NMR spectra of 3,3-dimethylpiperidine (1) at -70 to 30 ℃ exhibit gradual change from slow to rapid exchange between two alternate chair forms. The exchange rate constant was determined as a function of temperature by simulating the line shape of the signal from the two methyl groups using the modified Bloch equations. The resulting free energy of activation is ΔG* = 44.4±1.9 kJ mol-1 at 298 K. The 1H NMR spectrum of a D2O or dimethylsulfoxide-d6 (DMSO-d6) solution containing 1 and [SiW11CoⅡO39]6- exhibits separate signals for the free ligand and the complex, indicating that the ligand exchange is slow on the NMR time scale. In D2O the piperidine ring is frozen as a chair form even at room temperature with the cobalt ion bonded to the axial position of the nitrogen atom. When DMSO-d6 is added to the D2O solution, the NMR spectral change suggests that a rapid exchange occurs between the chair form and another conformer. It is proposed that the conformation of ^b1^b coordinated to [SiW11CoⅡO39]6- in DMSO-d6 is close to a twist form.

Cloning, Purification, and Structural Characterization by 1D 1H-NMR of the PDZ domain of the Shank3 protein (Shank3 PDZ 도메인의 동정, 정제 및 1차 NMR 구조분석)

  • Sung, Mee-Sook
    • Journal of Life Science
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    • v.17 no.3 s.83
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    • pp.345-349
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    • 2007
  • We wished to create a set of small molecular weight PDZ domain ligands that may be used in functional studies on the proteins AF6, PSD-95 and Shank. As a starting point, the Shank3 PDZ domain was cloned, purified, and characterized the structure of Shank3 PDZ domain by 1D $^1H-NMR$. The chemical shift dispersion of the proton signals indicates that the purified Shank3 PDZ protein is very pure and globally well folded. Currently, we are working on improving the yield of the protein production for complete NMR structural analysis of the Shank3 PDZ domain.

Complete Assignment of $^1H$- and $^{13}C-NMR$ in (20R)-panaxadiol and (20R)-panaxatriol ((20R)-파낙사디올과 (20R)-파낙사트리올에 대한 $^1H$- 및 $^{13}C-NMR$의 완전동정)

  • Kim, Dong-Seon;Baek, Nam-In;Park, Jong-Dae;Lee, You-Hui;Kim, Shin-Il
    • YAKHAK HOEJI
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    • v.40 no.3
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    • pp.293-299
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    • 1996
  • The $^1H$- and $^{13}C$-NMR signals of (20R)-panaxadiol and (20R)-panaxatriol were completely assigned by the extensive application of modern 2D-NMR techniques, $^1H-^1H$ COSY, HMQC and HMBC.

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

  • 이헌주;정춘수;강사욱;하영칠
    • Korean Journal of Microbiology
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    • v.27 no.1
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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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Establishment of a Simple and Rapid Method for Quantitative Determination of -Aminobutyric Acid Using 1H NMR and Production of γ-Aminobutyric Acid in Cell Suspension Cultures of Coriandrum sativum L. (1H NMR에 의한 γ-Aminobutyric Acid의 간단하고 신속한 정량분석법 확립과 고수 (Coriandrum sativum L.) 현탁배양세포로부터 γ-Aminobutyric Acid의 생산)

  • Kim, Suk-Weon;Liu, Jang-R.
    • Journal of Plant Biotechnology
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    • v.34 no.3
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    • pp.207-212
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    • 2007
  • This study describes a simple and rapid method for quantitative determination of $\gamma$-aminobutyric acid (GABA) using $^1H$ NMR spectroscopy from whole cell extracts of plant suspension cultures. When 9 cell lines derived from 8 species of higher plants maintained in liquid Marashige and Skoog (MS) medium supplemented with 1 mg/L 2,4-dichlorophenoxyacetic acid (2,4-D) were subjected to $^1H$ NMR, a cell line of Coriandrum sativum L. exhibited the highest level of GABA. The level reached up to 16.9 mg/dry wt when cells were cultured in MS medium supplemented with 0.5 mg/L 2,4-D after 3 weeks of incubation. The method for quantitative determination of GABA using $^1H$ NMR established in this study could be applied to high-throughput screening of various plant resources for GABA production and the cell suspension culture system of C. sativum could be further developed for commercial production of GABA.