• Title/Summary/Keyword: NMR Analysis

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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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    • v.17 no.3
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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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    • v.33 no.5
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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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    • v.17 no.2
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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
    • Journal of the Korean Magnetic Resonance Society
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    • v.8 no.2
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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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Chemical Structure Study on Copolyterephthalates Based on Ethylene Glycol and 1, 4-Cyclohexane Dimethanol by High Resolution NMR Analysis (고분해능 NMR 분석법에 의한 에틸렌글리콜과 1, 4-시클로헥산디메탄올의 테레프탈산 공중합체의 화학구조 연구)

  • Yoo, Hee-Yeoul;Kim, Sang-Wook;Okui, Norimasa
    • Applied Chemistry for Engineering
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    • v.4 no.4
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    • pp.770-775
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    • 1993
  • Chemical structure of poly(ethylene terephthalate-co-1, 4-cyclohexylene dimethylene terephthalate), P(ET-CT) copolyesters was investigated by High Resolution NMR analysis. The copolymer composition and isomeric ratio were determined by methylene resonance peaks which were separated into three peaks corresponding to ET, trans CT and cis CT units, respectively. The copolymer sequence distribution was evaluated from the carbon resonance peaks connected to carbonyl groups in benzene, indicating died distribution. According to statistics model, these copolyesters are almost random copolymers. The copolymer sequence distribution could be simulated and its averaged length was calculated by random copolymer statistics.

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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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    • v.34 no.3
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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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    • v.34 no.5
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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.