• Title/Summary/Keyword: $^2H$ 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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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.

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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Role of NH4 and H2O in Tutton Salt (NH4)2M(SO4)2·6H2O (M=Fe and Zn) Single Crystals Studied by 1H and 14N NMR at High Temperatures

  • Park, Sung Soo;Lim, Ae Ran
    • Journal of the Korean Magnetic Resonance Society
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    • v.21 no.2
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    • pp.67-71
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    • 2017
  • At high temperature, the roles of $NH_4$ and $H_2O$ in $(NH_4)_2Fe(SO_4)_2{\cdot}6H_2O$ and $(NH_4)_2Zn(SO_4)_2{\cdot}6H_2O$ single crystals were investigated using a pulse NMR spectrometer. Temperature was shown to have a significant influence, causing changes in the deformation of $NH_4$ and $H_2O$. From the $^1H$ NMR and $^{14}N$ NMR spectrum, the forms of environment surrounding $^{14}N$ in $NH_4$ groups is more important than the loss of $H_2O$ groups. NMR studies indicate that $NH_4{^+}$ ions in Tutton salts play an important role in the changes of the crystal structure at high temperatures.

Ferroelectric-Paraelectric Phase Transition of CsH2PO4 studied by Static NMR and MAS NMR

  • Lim, Ae Ran;Lee, Kwang-Sei
    • Journal of the Korean Magnetic Resonance Society
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    • v.19 no.1
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    • pp.29-35
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    • 2015
  • The microscopic dynamics of $CsH_2PO_4$, with two distinct hydrogen bond lengths, are studied by static nuclear magnetic resonance (NMR) and magic angle spinning (MAS) NMR. The proton dynamics of the two crystallographically inequivalent hydrogen sites were discussed in terms of the $^1H$ NMR and $^1H$ MAS NMR spectra. Although the hydrogen bonds have two inequivalent sites, H(1) and H(2), distinct proton dynamics for the two sites were not found. Further, the $^{133}Cs$ spectrum is more or less continuous near $T_{C1}$ (=153 K). Finally, the phase transition mechanism of $T_{C1}$ in $CsH_2PO_4$ is related to the ordering of protons.

Hot-Pressing Effects on Polymer Electrolyte Membrane Investigated by 2H NMR Spectroscopy

  • Lee, Sang Man;Han, Oc Hee
    • Bulletin of the Korean Chemical Society
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    • v.34 no.2
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    • pp.510-514
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    • 2013
  • The structural change of Nafion polymer electrolyte membrane (PEM) induced by hot-pressing, which is one of the representative procedures for preparing membrane-electrode-assembly for low temperature fuel cells, was investigated by $^2H$ nuclear magnetic resonance (NMR) spectroscopy. The hydrophilic channels were asymmetrically flattened and more aligned in the membrane plane than along the hot-pressing direction. The average O-$^2H$ director of $^2H_2O$ in polymer electrolyte membrane was employed to extract the structural information from the $^2H$ NMR peak splitting data. The dependence of $^2H$ NMR data on water contents was systematically analyzed for the first time. The approach presented here can be used to understand the chemicals' behavior in nano-spaces, especially those reshaping and functioning interactively with the chemicals in the wet and/or mixed state.

Analytical Study for an Acrylic Coating (아크릴 코팅의 성분 분석 연구)

  • Kim, Seog-Jun
    • Analytical Science and Technology
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    • v.17 no.2
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    • pp.98-107
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    • 2004
  • In this study, $^1H$ NMR spectroscopy and HPLC were used to identify the type and quantity of each component in an acrylic coating materials applied for an automotive part. By the $^1H$ NMR analysis, it was found that this acrylic coating contained about 88.40 wt% of poly methyl methacrylate (PMMA), 7.05 wt% of methyl methacrylate (MMA), and 2.36 wt% of allyl methacrylate. Polymer additives such as a benzotriazole light stabilizer (Hisorb 328), an oxanilide light stabilizer, butylated hydroxy toluene (BHT), and dimethyl phthalate (DMP) were also identified and measured quantitatively from the $^1H$ NMR spectra. However, only two light stabilizers were identified by reverse phase (RP) HPLC analysis using Bondapak C18 column, methanol mobile phase, and a PDA (Photodiode array) detector. The contents of two light stabilizers in the acrylic coating were measured by a quantitative analysis through UV-Vis spectroscopy and compared with the NMR data. The analytical informations from $^1H$ NMR spetra were better than those from HPLC-PDA plot.

Structural characteristics of [N(CH3)4]2CdCl4 determined by 1H MAS NMR, 13C CP/ MAS NMR, and 14N NMR

  • Lee, Seung Jin;Lim, Ae Ran
    • Journal of the Korean Magnetic Resonance Society
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    • v.19 no.1
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    • pp.18-22
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    • 2015
  • The structural geometry of $[N(CH_3)_4]_2CdCl_4$ in a hexagonal phase is studied by $^1H$ MAS NMR, $^{13}C$ CP/MAS NMR, and $^{14}N$ NMR. The changes in the chemical shifts for $^{13}C$ and $^{14}N$ in the hexagonal phase are explained by the structural geometry. In addition, the temperature dependencies of the spin-lattice relaxation time in the rotating frame $T_{1{\rho}}$ for $^1H$ MAS NMR and $^{13}C$ CP/MAS NMR are measured.

Quantitative Analysis of Paeoniflorin from Paeonia lactiflora Using $^1H-NMR$

  • Yoo, Jong-Su;Song, Myoung-Chong;Ahn, Eun-Mi;Lee, Youn-Hyung;Rho, Yeong-Deok;Baek, Nam-In
    • Natural Product Sciences
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    • v.12 no.4
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    • pp.237-240
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    • 2006
  • Paeoniflorin, the major component of the root of Paeonia lactiflora, was quantitatively analyzed using $^1H-NMR$ spectrometry. The quantity of paeoniflorin was calculated by the ratio of the intensity of the signals (H-9, H-10, H-2', 6') to the aldehyde peak of the known amount of internal standard, 2,4,6-trihydroxybenzaldehyde. These results were compared with the conventional HPLC method. The contents of paeoniflorin in P. lactiflora, which were respectively calculated by H-9, H-10, H-2', 6' in the $^1H-NMR$ spectra and HPLC, were determined $2.60{\pm}0.07,\;2.44{\pm}0.09,\;2.77{\pm}0.12\;and\;2.46{\pm}0.16%$. 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 paeoniflorin with an analysis time for only 20 min without any preprocessing.

$^1/H-NMR$ and NOE Studies of 2-Cephems and 3-Cephems

  • Im, Chae-Uk;Yim, Chul-Bu;Micetich, Ronald-G.;Mohsen, Daneshtalab
    • Archives of Pharmacal Research
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    • v.20 no.6
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    • pp.652-655
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    • 1997
  • $^{1}H-NMR$ signals of 2-cephems and 3-cephems have been assigned and the Nuclear Overhauser Effect (NOE) study of these compounds was undertaken.

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