• 제목/요약/키워드: NMR analysis

검색결과 1,402건 처리시간 0.029초

Quantitative Analysis of Coumarins from Angelica gigas Using $^1H$-NMR

  • Yoo, Jong-Su;Ahn, Eun-Mi;Song, Myoung-Chong;Bang, Myun-Ho;Kim, Dong-Hyun;Han, Min-Woo;Kwak, Ho-Young;Lee, Dae-Young;Lyu, Ha-Na;Baek, Nam-In
    • Food Science and Biotechnology
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    • 제17권3호
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    • pp.573-577
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    • 2008
  • $^1H$-Nuclear magnetic resonance (NMR) spectrometry was applied to the quantitative analysis of coumarins in the roots of Angelica gigas without any chromatographic purification. The experiment was performed by the analysis of each singlet germinal methyl, which was well separated in the range of 1.0-2.0 ppm in the $^1H$-NMR spectrum. The quantity of the compounds was calculated by the ratio of the intensity of each compound to the known amount of internal standard (dimethyl terephthalate). These results were compared with the conventional gas chromatography (GC) method. The contents of decursin and decursinol angelate in A. gigas were determined $1.98{\pm}0.07$, $1.13{\pm}0.08%$ in quantitative $^1H$-NMR method and $2.06{\pm}0.24$, $1.17{\pm}0.24%$ in GC method, respectively. 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 coumarins with an analysis time for only 10 min without any preprocessing.

Developing 500 MHz NB 19F-13C Double Resonance Solid-State NMR Probe for in-situ Analysis of Liquid Crystal Display Panels

  • Choi, Sung-Sub;Jung, Ji-Ho;Park, Yu-Geun;Park, Tae-Joon;Park, Gregory Hyung-Jin;Kim, Yong-Ae
    • Bulletin of the Korean Chemical Society
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    • 제33권5호
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    • pp.1577-1580
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    • 2012
  • The orientational and dynamic behavior of liquid crystal molecules on the alignment layer surfaces of liquid crystal display (LCD) devices is crucial to their performance, but there are only a few methods of experimentally elucidating the interactions between the liquid crystals and the alignment layers. Inspired by the natural and technical similarities between membrane proteins in lipid bilayers and liquid crystals in LCDs, we employed solid-state NMR methodologies originally developed for the study of membrane proteins in lipid bilayers for the in-situ analysis of liquid crystal display panels. In this article, we present a home-built 500 MHz narrowbore (NB) The orientational and dynamic behavior of liquid crystal molecules on the alignment layer surfaces of liquid crystal display (LCD) devices is crucial to their performance, but there are only a few methods of experimentally elucidating the interactions between the liquid crystals and the alignment layers. Inspired by the natural and technical similarities between membrane proteins in lipid bilayers and liquid crystals in LCDs, we employed solid-state NMR methodologies originally developed for the study of membrane proteins in lipid bilayers for the in-situ analysis of liquid crystal display panels. In this article, we present a home-built 500 MHz narrowbore (NB) $^{19}F-^{13}C$ double resonance solid-state NMR probe with a flat-square coil and the first application of this probe for the in-situ analysis of LCD panel samples. double resonance solid-state NMR probe with a flat-square coil and the first application of this probe for the in-situ analysis of LCD panel samples.

Fingerprinting Differentiation of Astragalus membranaceus Roots According to Ages Using 1H-NMR Spectroscopy and Multivariate Statistical Analysis

  • Shin, Yoo-Soo;Bang, Kyong-Hwan;In, Dong-Su;Sung, Jung-Sook;Kim, Seon-Young;Ku, Bon-Cho;Kim, Suk-Weon;Lee, Dong-Ho;Choi, Hyung-Kyoon
    • Biomolecules & Therapeutics
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    • 제17권2호
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    • pp.133-137
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    • 2009
  • The root of Astragalus membranaceus is a traditional folk medicine that has been used for many therapeutic purposes in Asia. It reportedly acts as an immunostimulant, tonic, hepatoprotective, diuretic, antidiabetic, analgesic, expectorant, sedative, and anticancer drug. In this study, metabolomic profiling was applied to the roots of A. membranaceus of different ages using NMR coupled with two multivariate statistical analysis methods: such as principal components analysis (PCA) and canonical discriminant analysis (CDA). This allowed various metabolites to be assigned in NMR spectra, including $\gamma$-aminobutyric acid (GABA), aspartic acid, succinic acid, glutamic acid, glutamine, N-acetyl aspartic acid, acetic acid, arginine, alanine, threonine, lactic acid, and valine. The score plot from PCA and also CDA allowed a clear separation between samples according to age.

NMR study on secondary metabolites isolated from an identified tunicate

  • Rho, Jung-Rae
    • 한국자기공명학회논문지
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    • 제8권2호
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    • pp.115-126
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    • 2004
  • Four secondary metabolites from an unidentified tunicate were isolated by treatment with trichloroethyl chloroformate(TECF) or acetic anhydride in pyridine. Their structures were determined by an extensive NMR analysis and the configuration of diacetyl derivatives(3a, 4a) was assigned by comparing with NMR data of a similar compound. Three new naturally occurring compounds (1, 3, 4) showed potent brine shrimp lethality and antifungal effect against Candia albicans.

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고분해능 NMR 분석법에 의한 에틸렌글리콜과 1, 4-시클로헥산디메탄올의 테레프탈산 공중합체의 화학구조 연구 (Chemical Structure Study on Copolyterephthalates Based on Ethylene Glycol and 1, 4-Cyclohexane Dimethanol by High Resolution NMR Analysis)

  • 유희열;김상욱
    • 공업화학
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    • 제4권4호
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    • pp.770-775
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    • 1993
  • 에틸렌글리콜과 1, 4-시클로헥산디메탄올의 테레프탈산 공중합체인, poly(ethylene terephthalate-co-1, 4-cyelohexylene dimethylene terephthalate), P(ET-CT)의 화학 구조를 고분해능 NMR 분석을 통하여 조사하였다. $^1H$ NMR 분석에서 메칠렌기에 의한 chemical shift가 ET, 트란스 CT, 및 시스 CT로 분리됨에 따라 공중합조성 및 이성질체의 비율을 구할 수 있었다. $^{13}C$ NMR 분석에서 카르보닐기에 연결된 벤젠기의 탄소가 diad로 분리됨에 따라 공중합 연쇄 분포(copolymer sequence distribution)를 구한 결과, P(ET-CT) 공중합체는 랜덤공중합체임이 판명되었다. 아울러 랜덤 통계식을 이용하여 공중합 연쇄의 분포 및 평균길이를 구할 수 있었다.

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Low-ε Static Probe Development for 15N-1H Solid-state NMR Study of Membrane Proteins for an 800 MHz NB Magnet

  • Park, Tae-Joon;Choi, Sung-Sub;Jung, Ji-Ho;Park, Yu-Geun;Kim, Yongae
    • Bulletin of the Korean Chemical Society
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    • 제34권3호
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    • pp.823-826
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    • 2013
  • A low-${\varepsilon}$ solid-state NMR(Nuclear Magnetic Resonance) probe was developed for the spectroscopic analysis of two-dimensional $^{15}N-^1H$ heteronuclear dipolar coupling in dilute membrane proteins oriented in hydrated and dielectrically lossy lipid environments. The system employed a 800 MHz narrow-bore magnet. A solenoid coil strip shield was used to reduce deleterious RF sample heating by minimizing the conservative electric fields generated by the double-tuned resonator at high magnetic fields. The probe's design, construction, and performance in solid-state NMR experiments at high magnetic fields are described here. Such high-resolution solid-state NMR spectroscopic analysis of static oriented samples in hydrated phospholipid bilayers or bicelles could aid the structural analysis of dilute biological membrane proteins.

Study of Metabolic Profiling Changes in Colorectal Cancer Tissues Using 1D 1H HR-MAS NMR Spectroscopy

  • Kim, Siwon;Lee, Sangmi;Maeng, Young Hee;Chang, Weon Young;Hyun, Jin Won;Kim, Suhkmann
    • Bulletin of the Korean Chemical Society
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    • 제34권5호
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    • pp.1467-1472
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    • 2013
  • Metabolomics is a field that studies systematic dynamics and secretion of metabolites from cells to understand biological pathways based on metabolite changes. The metabolic profiling of intact human colorectal tissues was performed using high-resolution magic angle spinning (HR-MAS) NMR spectroscopy, which was unnecessary to extract metabolites from tissues. We used two different groups of samples, which were defined as normal and cancer, from 9 patients with colorectal cancer and investigated the samples in NMR experiments with a water suppression pulse sequence. We applied target profiling and multivariative statistical analysis to the analyzed 1D NMR spectra to identify the metabolites and discriminate between normal and cancer tissues. Cancer tissue showed higher levels of arginine, betaine, glutamate, lysine, taurine and lower levels of glutamine, hypoxanthine, isoleucine, lactate, methionine, pyruvate, tyrosine relative to normal tissue. In the OPLS-DA (orthogonal partial least square discriminant analysis), the score plot showed good separation between the normal and cancer groups. These results suggest that metabolic profiling of colorectal cancer could provide new biomarkers.

Application of metabolic profiling for biomarker discovery

  • Hwang, Geum-Sook
    • 한국응용약물학회:학술대회논문집
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    • 한국응용약물학회 2007년도 Proceedings of The Convention
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    • pp.19-27
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    • 2007
  • An important potential of metabolomics-based approach is the possibility to develop fingerprints of diseases or cellular responses to classes of compounds with known common biological effect. Such fingerprints have the potential to allow classification of disease states or compounds, to provide mechanistic information on cellular perturbations and pathways and to identify biomarkers specific for disease severity and drug efficacy. Metabolic profiles of biological fluids contain a vast array of endogenous metabolites. Changes in those profiles resulting from perturbations of the system can be observed using analytical techniques, such as NMR and MS. $^1H$ NMR was used to generate a molecular fingerprint of serum or urinary sample, and then pattern recognition technique was applied to identity molecular signatures associated with the specific diseases or drug efficiency. Several metabolites that differentiate disease samples from the control were thoroughly characterized by NMR spectroscopy. We investigated the metabolic changes in human normal and clinical samples using $^1H$ NMR. Spectral data were applied to targeted profiling and spectral binning method, and then multivariate statistical data analysis (MVDA) was used to examine in detail the modulation of small molecule candidate biomarkers. We show that targeted profiling produces robust models, generates accurate metabolite concentration data, and provides data that can be used to help understand metabolic differences between healthy and disease population. Such metabolic signatures could provide diagnostic markers for a disease state or biomarkers for drug response phenotypes.

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