• Title/Summary/Keyword: 1D/2D-NMR

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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.

Structure Determination of Sucrose by Acetylation and Acid Hydrolysis

  • Min, Hee-Jeong;Lee, Tae-Seong;Bae, Young-Soo
    • Journal of the Korean Wood Science and Technology
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    • v.42 no.2
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    • pp.183-192
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    • 2014
  • For the structure determination of D-(+)-sucrose, which consists of ${\alpha}$-D-(+)-glucose and ${\beta}$-D-(+)-fructose, it was acetylated with acetic anhydride and triethyl amine, pyridine, zinc chloride, and sodium acetate as catalysts. The acetylated D-(+)-sucrose was acid-hydrolyzed using sulfuric acid and sodium chloride in methanolic solution. The structures of the reaction products were determined by $^1H$-NMR and $^{13}C$-NMR spectra. The yield of the acetylation indicated the high value in zinc chloride as 70% in zinc chloride catalyst. The acid-hydrolyzed product of the acetylated D-(+)-sucrose, 2,3,4,6,1',3',4',6'-octa-O-acetyl-D-(+)-sucrose, gave 2,3,4,6-tetra-O-acetyl-${\beta}$-D-(+)-glucose and it suggests that the acetylated D-(+)-sucrose was rearranged through the formation of oxonium ion by mutarotation in the 2,3,4,6-tetra-O-acetyl-${\alpha}$-D-(+)-glucose moiety and through the ring opening in the 1',3',4',6'-tetra-O-acetyl-${\beta}$-D-(+)-fructose moiety.

A New Flavonoid from Carrichtera annua

  • Shahat, Abdelaaty A.;Abdel-Shafeek, Khaled A.;Husseiny, Husseiny A.;Claeys, Magda;Apers, Sandra;Pieters, Luc
    • Natural Product Sciences
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    • v.12 no.3
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    • pp.122-124
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    • 2006
  • Three flavonoid glycosides, $kaempferol-3-O-{\alpha}-L-rhamnopyranosyl-(1\;{\rightarrow}\;6)-{\beta}$-D-glucopyranoside$ or kaempferol-3-O-rutinoside (1), $isorhamnetic-3-O-{\alpha}-L-rhamnopyranosyl-(16)-{\beta}-D-glucopyranoside$ or isorhamnetin-3-O-rutinoside (2), and $quercetin-3-O-{\beta}-D-glucopyranosyl-(1 ${\rightarrow}\;2)-{\beta}-L-arabinopyranoside$ 3, the latter one being a new compound, were isolated from the methanolic extract of the aerial parts of Carrichtera annua. Mass spectrometry and 1D and 2D NMR spectroscopy allowed establishing the structure of these compounds.

Construction of 1H-15N Double Resonance Solid-State NMR Probe for Membrane Proteins in Aligned Bicelles

  • Park, Tae-Joon;Kim, Ji-Sun;Um, Seung-Hoon;Kim, Yong-Ae
    • Bulletin of the Korean Chemical Society
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    • v.31 no.5
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    • pp.1187-1191
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    • 2010
  • $^1H-^{15}N$ heteronuclear dipolar coupling solid-state NMR experiments on lipid bilayer or bicelle samples are very useful for the structural studies of membrane proteins. However, to study these biological samples using solid-state NMR, a specific probe with high efficiency and high capability is required. In this paper, we describe the optimized design, construction, and efficiency of a 400 MHz wide-bore $^1H-^{15}N$ solid-state NMR probe with 5-mm solenoidal rf coil for high power, multi-pulse sequence experiments, such as 2D PISEMA or 2D SAMMY.

Tone Quality Improvement Algorithm using Intelligent Estimation of Noise Pattern (잡음 패턴의 지능적 추정을 통한 음질 개선 알고리즘)

  • Seo, Joung-Kook;Cha, Hyung-Tai
    • Journal of the Korean Institute of Intelligent Systems
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    • v.15 no.2
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    • pp.230-235
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    • 2005
  • In this paper, we propose an algorithm that improves a tone quality of a noisy audio signal in order to enhance a performance of perceptual filter using intelligent estimation of noise pattern from a band degraded by additive noise. The proposed method doesn't use the estimated noise which is obtained from silent range. Instead new estimated noise according to the power of signal and effect of noise variation is considered for each frame. So the noisy audio signal is enhanced by the method which controls a estimation of noise Pattern effectively in a noise corruption band. To show the performance of the proposed algorithm, various input signals which had a different signal-to-noise ratio(SNR) such as $5\cal{dB},\;10\cal{dB},\;15\cal{dB}\;and\;20\cal{dB}$ were used to test the proposed algorithm. we carry out SSNR and NMR of objective measurement and MOS test of subjective measurement. An approximate improvement of $7.4\cal{dB},\;6.8\cal{dB},\;5.7\cal{dB},\;5.1\cal{dB}$ in SSNR and $15.7\cal{dB},\;15.5\cal{dB},\;15.2\cal{dB},\;14.8\cal{dB}$ in NMR is achieved with the input signals, respectively. And we confirm the enhancement of tone quality in terms of mean opinion score(MOS) test which is result of subjective measurement.

Application of multi dimensional NMR experiments to VBS RNAs of Yeast Saccaromyces cerevisiae virus

  • Chaejoon Cheong;Cheong, Hae-Kap;Yoo, Jun-Seok
    • Journal of the Korean Magnetic Resonance Society
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    • v.5 no.1
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    • pp.29-36
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    • 2001
  • The structures of two VBS (viral binding site) RNAs, SL1 and SL2, of Yeast Saccharomyces cerevisiae vims have been studied by 2D and 3D NMR experiments. VBSs play a crucial role in viral particle binding to the plus strand and packaging of the RNA. The secondary structures of the two VBS RNAs share a common feature of the stem-internal loop-stem-hairpin loop structure although the size of the internal loops of SL1 and SL2 differs. 2D experiments were sufficient for fill assignments of SL1. However, isotope labeling of the sample and multidimensional experiments were required for 28-nucleotide-long SL2 due to the spectral overlap. Several 3D HCCH experiments have accomplished full assignment of SL2 RNA.

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Micelle Formation of Surfactant Solution(3) -Self-Diffusion and 1H Relaxation for Mixed Micelle of Nonionic and Ionic Surfactants- (계면활성제 수용액에서 미셀형성(제3보) -비이온성과 이온성계면활성제의 혼합 미셀에 있어 자기확산 및 프로톤 이완-)

  • Choi, Seung-Ok;Kwack, Kwang-Soo;Park, Heung-Jo;Nam, Ki-Dae
    • Applied Chemistry for Engineering
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    • v.10 no.6
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    • pp.876-880
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    • 1999
  • The surfactant self-diffusion coefficients of mixed micellar solutions of ionic and nonionic surfactants have been measured by the NMR pulsed field gradient spin echo(FT-PGSE) method. In addition, the line widths of $^1H$ NMR signal have been monitored. The system investgated are $C_{12}EO_5/SDS/D_2O$, $C_{12}EO_5/DTAC/D_2O$, and $C_{12}EO_8/SDS/D_2O$. In the sample series, the molar ratios of $D_2O$ to surfactant(ionic+nonionic) were kept constant while the surfactant mixing ratio was varied. For the $C_{12}EO_5$ system, the surfactant self-diffusion coefficient indicates minimum when the surfactant mixing ratio is about 20% ionic surfactant. The observed decrease in self-diffusion coefficients as nonionic surfactant was replaced by ionic surfactant is interpreted to mainly be due to an increased micelle-micelle repulsion. The increase in self-diffusion coefficients occurring at higher fraction of ionic surfactant is shown to be due to a decrease in micelle size. For the $C_{12}EO_8$ system, the effect of the surfactant mixing ratio is much weaker which can be understood by considering the molecular geometry and large headgroup area. The proton NMR line widths correlate well with the self-diffusion coefficients and broadening of the alkyl chain methylene signals is found when the self-diffusion coefficients is low.

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A new derivative of phorbaketals isolated from a Marine Sponge Phorbas species

  • Hwang, Buyng-Su;Yang, Cao;Rho, Jung-Rae
    • Journal of the Korean Magnetic Resonance Society
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    • v.15 no.2
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    • pp.128-136
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    • 2011
  • A new sesterterpenoid, phorbaketal derivative, was isolated from the marine sponge Phorbas species. Its planar structures was completely determined from a combination of extensive 1D and 2D NMR experiments and MS data, and also the stereochemistry on the chiral centers were established by the ROESY experiment and the comparison with the $^1H$ and $^{13}C$ chemical shifts of the known phorbaketal compounds. This compound 1 moderately showed cytotoxicity effect against hepatoma cancer HepG2 cell.

Spirostane-type steroidal saponin from Allium hookeri roots with mushroom tyrosinase inhibitory activity

  • Kim, Yun Na;Lee, Jae Sun;Ock, Kwang Ju;Jeong, Eun Ju
    • Journal of the Korean Magnetic Resonance Society
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    • v.23 no.4
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    • pp.87-92
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    • 2019
  • Allium hookeri (Liliaceae) has been received the increasing attention as a bioactive resource due to its potent biological activities including anti-oxidant, anti-obesity, anti-microbial and lipid-regulating activities. The beneficial effects of A. hookeri are known contributed from the high content of organosulfur compounds in A. hookeri. Though a variety of articles demonstrated that A. hookeri contains 'saponin' as a bioactive constituent, the scientific evidence to prove it was limited. In the present study, we have attempted to identify saponin contained in A. hookeri through chromatographic isolation and NMR spectroscopic methods. As a result, a spirostane-type steroidal saponin (1) has been successfully isolated from the methanolic extract of A. hookeri roots. The structure of 1 was elucidated by extensive 1D and 2D spectroscopic methods including 1H-NMR, 13C-NMR, 1H-1H COSY, HSQC, HMBC and NOESY; identified as (3β, 22R, 25S)-spirost-5-en-3yl O-6-deoxy-α-L-mannopyranosyl-(1→4)-O-6-deoxy-α-L-mannopyranosyl-(1→4)-O-[6-deoxy-α-L-mannopyranosyl-(1→2)]-β-D-gluco pyranoside. 1 showed the significant inhibitory activity on mushroom tyrosinase with IC50 values of 248.7 μM while the inhibition on alpha-glucosidase was not significant.

Isolation and structure elucidation of a catechin glycoside with phospholipase $A_2$ inhibiting activity from Ulmi cortex

  • Park, Sunghyouk;Goo, Yang-Mo
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1995.04a
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    • pp.58-58
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    • 1995
  • 식물에서부터 새로운 소염작용제를 개발하기 위하여 여러식물을 대상으로 염증반응의 초기단계에서 중요한 역할을 하는 것으로 알려진 Phospholipase $A_2$에 저해활성을 갖는 물질을 검색하였고 그 중 강한 억제활성을 보인 유근피에서 유효성분을 분리하였다. 유근피의 에칠 아세테이트 분획에 대하여 실리카겔 크로마토그래피, Sephadex LH-20 크로마토그래피, 분취 박막 크로마토그래피를 수행하여 phenol성 -OH기를 갖는 활성성분인 PSH-II-84-1를 분리하였다. $^1$H-NMR 신호의 양상과 짝지움 상수 값에서 분리된 물질은 (+)-catechin 의 당 유도체로 확인되었다. $^{13}$C-NMR 자료를 분석하여 치환된 당은 D-apiofuranose로 확인되었다. 방향족환의 $^{l3}$C-NMR 신호들은 extended Huekel theory를 응용하여 얻은 net charge 계산 값과 상관시켜 할당하였다. 이상의 구조연구 결과 이 물질은 (+)-catechin-7-0-$\beta$-D-apiofuranoside로 밝혀졌다. (+)-catechin-7-0-$\beta$-D-apiofuranoside의 효소억제활성은 Type II Phospholipase $A_2$에 대하여 $IC_{50}$/이 600$\mu$M이었다.다.

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