• Title/Summary/Keyword: NMR

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Identification of 1H-NMR characteristics for black ginger specimens from different places of origin

  • Kwon, Hyeok;Lee, Sojung;Hong, Sukyung;Kiyonga, Alice Nguvoko;Yi, Jong-Jae;Jung, Kiwon;Son, Woo Sung
    • Journal of the Korean Magnetic Resonance Society
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    • v.23 no.4
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    • pp.93-97
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    • 2019
  • Black ginger (Kaempferia parviflora) is a short-lived ginger plant with dark purple colored root and is known to be effective in treating diabetes and obesity. To find out the difference in the characteristics of the black ginger according to the variety of production, 1D proton NMR experiments were performed on 4 types of black gingers from different regions. The NMR spectra of all black ginger showed the characteristic peaks of the polymethoxy flavone compounds, and the chemical shifts and intensity of peaks showed slight differences depending of the type of black ginger implying the difference in molecular environment. These initial NMR experiments can be applied to the identification of the diversity of black ginger in physiological function according to the climate of regions using SNIF-NMR (Site-specific Natural Isotope Fractionation studied by NMR).

Structural nature of chemically inequivalent borons in the nonlinear optical material β-BaB2O4 studied using 11B MAS NMR and 11B single-crystal NMR

  • Kim, Woo Young;Lim, Ae Ran
    • Journal of the Korean Magnetic Resonance Society
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    • v.17 no.2
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    • pp.86-91
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    • 2013
  • Detailed information about the structural nature of three-coordinate borons in ${\beta}-BaB_2O_4$ is obtained through $^{11}B$ MAS NMR and $^{11}B$ single-crystal NMR. The three-coordinate $BO_3$ of the two borons B(1) and B(2) in ${\beta}-BaB_2O_4$ were distinguished. The spin-lattice relaxation time in the laboratory frame $T_1$ for B(1) and B(2) slowly decreases with increasing temperature, whereas the spin-lattice relaxation time in the rotating frame $T_{1{\rho}}$ for B(1) and B(2), which differs from $T_1$, is nearly constant. The B(1) and B(2) of the two types were distinguished by $^{11}B$ MAS NMR and $^{11}B$ single-crystal NMR.

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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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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Comparison of metabolic profiling of Daphnia magna between HR-MAS NMR and solution NMR techniques

  • Kim, Seonghye;Lee, Sujin;Lee, Wonho;Lee, Yujin;Choi, Juyoung;Lee, Hani;Li, Youzhen;Ha, Seulbin;Kim, Suhkmann
    • Journal of the Korean Magnetic Resonance Society
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    • v.25 no.2
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    • pp.12-16
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    • 2021
  • Daphnia magna is used as target organism for environmental metabolomics. The metabolome of D. magna was studied with NMR spectroscopy. Most studies used the extract of D. magna, but the reproducibility cannot be obtained using extracted sample. In this study, lyophilized D. magna samples were analyzed with two different 1H NMR techniques, HR-MAS on intact tissues and solution NMR on extracted tissues. Samples were measured three times using 600 MHz NMR spectrometer. Metabolite extraction required more than twice as many D. magna, but the metabolite intensity was lower in solution NMR. In the spectra of HR-MAS NMR, the lipid signal was observed, but they did not interfere with metabolite profiling. We also confirmed the effect of swelling time on signal intensities of metabolites in HR-MAS NMR, and the results suggest that appropriate swelling should be used in lyophilized D. magna to improve the accuracy of metabolite profiles.

Effect of Spinning Speed on 29Si and 27Al Solid-state MAS NMR Spectra for Iron-bearing Silicate Glasses (시료의 회전 속도가 함철 비정질 규산염의 고상 NMR 신호에 미치는 영향)

  • Kim, Hyo-Im;Lee, Sung Keun
    • Journal of the Mineralogical Society of Korea
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    • v.31 no.4
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    • pp.295-306
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    • 2018
  • Despite the utility of solid-state NMR, NMR studies of iron-bearing silicate glasses remain a challenge because the variations in the peak position and width with increasing iron content reflect both paramagnetic effect and iron-induced structural changes. Therefore, it is essential to elucidate the effect of temperature on the NMR signal for iron-bearing silicate glasses. Here, we report the $^{29}Si$ and $^{27}Al$ MAS NMR spectra for $(Mg_{0.95}Fe_{0.05})SiO_3$ and $Fe_2O_3$-bearing $CaAl_2Si_2O_8$ (anorthite) glasses with varying spinning speed to interpret the NMR spectra for iron-bearing silicate glasses. The increase in the spinning speed results in an increase in the sample temperature. The current NMR results allow us to understand the origins of the changes in NMR signal with increasing iron content and to provide information on the dipolar interaction between nuclear spins. The $^{29}Si$ NMR spectra for $(Mg_{0.95}Fe_{0.05})SiO_3$ glass and $^{27}Al$ NMR spectra for $Fe_2O_3$-bearing $CaAl_2Si_2O_8$ glasses show that the peak shape and position of iron-bearing glasses do not change with increasing spinning speed up to 30 kHz. These results suggest that the NMR signal in the Fe-bearing glasses may stem from the 'survived nuclear spins' beyond the cutoff radius from the Fe, not from the paramagnetic shift. Based on the current results, the observed apparent shifts toward lower frequency of Al peak for $Fe_2O_3$-bearing $CaAl_2Si_2O_8$ glasses with increasing $Fe_2O_3$ at all spinning speed (15 kHz to 30 kHz) indicate the increase in the fraction of ${Q^4}_{Al}$(nSi) with lower n (i.e., 1 or 2) with increasing $Fe_2O_3$ and the spatial proximity between Fe and ${Q^4}_{Al}$(nSi) with higher n (i.e., 3 or 4). The present results show that changes in the NMR signal for iron-bearing silicate glasses reflect the actual iron-induced structural changes. Thus, it is clear that the applications of solid-state NMR for iron-bearing silicate glasses hold strong promise for unraveling the atomic structure of natural silicate glasses.

Comparison of in Vivo, in Vitro 3T MR Spectroscopy and Proton NMR Spectroscopy for the Fluid from Cystic Tumor: Preliminary Study (낭성 종양의 체액에 대한 생체내, 생체외 3T 양성자 자기공명분 광법과 양성자 핵자기공명기법의 비교: Preliminary Study)

  • Lee, Hui-Joong;Kim, Jong-Yeol;Chang, Yong-Min
    • Investigative Magnetic Resonance Imaging
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    • v.12 no.2
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    • pp.107-114
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    • 2008
  • Purpose : The aim of this study is to determine possibility of application of in vivo proton ($^1H$) magnetic resonance spectroscopy (MRS) in distinguishing cystic mass arising around pancreas by comparison of in vivo MRS, in vitro MRS using 3T MR machine, based on nuclear magnetic resonance (NMR). Materials and Methods : We obtained spectra of in vivo MRS, in vitro MRS and NMR from abdominal mass arising around pancreas (mucinous cystic neoplasm=5, intraductal papillary mucin producing tumor=5, pseudocyst=1, and lymphangioma=1). We estimated existence of peak of in vivo MRS, and in vitro MRS concordant to that of NMR. We also evaluated differential peak for predicting specific disease. Results : Correlation of presence of peak with NMR showed showed sensitivity of 29.6%, specificity of 82.6% and accuracy of 67.7% on in vivo MRS (p = 0.096, McNemar test), sensitivity of 57.1% and specificity of 92.6% and accuracy of 82.3% on in vitro MRS (p = 0.362, McNemar test). The spectra of NMR for IPMT showed more frequent peaks at 3.5-4.0 ppm (p=0.026). Conclusion : Although chemical analysis, using NMR could be regarded as possible tool to differentiate cystic masses, in vivo and in vitro MRS need further technical evolution for clinical application.

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Determination of phosphorous in lubricating oil by XRF and NMR methods (XRF 및 NMR 법에 의한 윤활유 중의 인 함량 비교분석 연구)

  • Lim, Heon-Sung;Han, Gee-Chung;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.18 no.2
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    • pp.168-172
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    • 2005
  • A comparison study of XRF and $^{31}P$-NMR method for the analysis of phosphorous in lubricating oil has been described. Pure oil and water were used for the observation of matrices effect variation by different analytical methods. Quantitative analysis was carried out by XRF and $^{31}P$-NMR using real samples. Significant difference is observed from the slopes on the calibration curves by the XRF due to the matrices (water: 124.0, oil: 276.6). While the result obtained from XRF showed a large matrix effect, the slopes obtained from $^{31}P$-NMR results of two different matrices, however, are in good agreement ranged of ${\pm}9%$ (water: 4.9, oil: 5.3).

Development of NMR Based Prototype Sensor for Non-destructive Sugar Content Measurement in Fruits. (수소 핵자기공명을 이용한 과실의 비괴적 당도측정 시작기의 개발)

  • 조성인;정창호
    • Journal of Biosystems Engineering
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    • v.21 no.3
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    • pp.336-342
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    • 1996
  • A 4.1MHz$1^H$ Nuclear Magnetic Resonance(NMR) sensor was designed and manufactured to evaluate the internal quality of fruits. The magnet console having 963gauss magnetic field induction was used for the NMR sensor. To optimize and evaluate the NMR sensor, glycerol and sugar-water solutions were used. $^1$H(proton) resonance signals were used to estimate the sugar contents in fruits. Artificial neural network models were developed to predict sugar contents in fruits from the proton resonance signals. The standard errors of prediction(SEP) were 0.565(apple), 0.394(pear) and 0.415(kiwi), respectively. The result implied that it was possible to evaluate apple, pear and kiwi into 3 grades using the NMR sensor.

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Development of Nondestructive Moisture Sensor for Agricultural Products Using Hydrogen NMR : Feasibility Experiments (수소자기공명원리를 이용한 비피괴적 농산물 함수율 측정장치 개발을 위한 기초실험)

  • Cho, S.I.
    • Journal of Biosystems Engineering
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    • v.18 no.3
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    • pp.252-261
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    • 1993
  • Nuclear magnetic resonance(NMR) was used to study a feasibility test for the possibility to develop a moisture sensor applicable for agricultural products such as raw and powdered grain. Samples of wheat flour and brown rice were tested with a 200MHz hydrogen NMR. The samples were loaded into 5mm NMR glass tubes and $30^{\circ}$ pulses were supplied to get resonance signals. Hydrogen spectrum intensities of the samples were compared to moisture content measured by a drying oven method. High linear correlations were obtained between the hydrogen spectrum intensity and moisture content. Therefore, moisure contents of agricultural products could be measured nondestructively utilizing the NMR principle. A low-cost design concept of the moisture sensor with the NMR principle was proposed for a practical use.

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