• Title/Summary/Keyword: H-NMR spectroscopy

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Extractives from the barks of Querus acutissima and Quercus variabilis (상수리나무(Querus acutissima)와 굴참나무(Querus vcariabilis) 수피의 추출성분)

  • 김진규;이상극;함연호;배영수
    • Journal of Korea Foresty Energy
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    • v.21 no.1
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    • pp.41-48
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    • 2002
  • The barks of oak trees (Quercus acutissima and Quercus variabilis) were collected, extracted with acetone-$H_2O$ (7:3, v/v), fractionated with hexane, $CH^2C1^2$ EtOAc and -$H_2O$, then freeze dried to give dark brown powder. The EtOAc soluble mixtures of the trees were chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-hexane mixture as eluents. The structures of isolated compounds were characterized by $^1H$, $^13C$ and 2D-NMR spectroscopy and molecular weights were determined by FAB-MS spectra. The isolated compounds from Quercus acutissima were (+)-catechin, (+)-gallocatechin, gallic acid and taxifolin-3-O-$\beta$-D-glucopyranoside and the compounds from Quercus variahilis (+)-catechin, caffeic acid and taxifolin-3-O-$\beta$-D-glucopyranoside.

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Identification of Anti-Oxidant and Anti-Tyrosinase Activity of Phenolic Components Isolated from Betula schmidtii (박달나무로부터 분리된 페놀성 화합물의 항산화 및 Tyrosinase 저해 활성 연구)

  • Wang, Da-Hye;Chung, Ha Sook
    • The Korean Journal of Food And Nutrition
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    • v.34 no.5
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    • pp.553-559
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    • 2021
  • The aim of study to investigate the phytochemicals and biological activities the bark of Betula schmidtii. The studies consisted of the solvent extraction, followed by the isolation of phenolic components 1~3 from ethyl acetate-soluble fraction of Betula schmidtii Bark. Their chemical structures were identified as arbutin (1), ρ-coumaric acid (2) and ferulic acid (3) using Ultraviolet-Visible (UV-Vis) Spectrophotometer, Electrospray Ionization Mass Spectrometry (ESI-MS) (negative ion mode), 1H-Nuclear Magnetic Resonance (NMR), 13C-NMR, 1H-1H Correlation Spectroscopy (COSY) and 1H-13C Hetero Nuclear Multiple Quantum Correlation (HMQC) spectral data. Compounds 1~3 shows the anti-oxidant effect with IC50 values of 29.74±1.52, 21.32±1.07 and 34.41±1.24 in 1,1-diphenyl-2-picrylhydrazyl (DPPH) free radical scavenging activity, respectively. Also, compounds 1~3 exhibited mushroom tyrosinase inhibitory activity with IC50 values of 31.14±1.07, 42.54±1.46 and 69.22±1.43 µM, respectively.

Purification and Characteristics of an Antibiotic Against MRSA form Streptomyces lydicus YSK-681 (Streptomyces lydicus YSK-681이 생산하는 메치실린 내성 황색 포도상구균에 유효한 항생물질의 정제 및 특성)

  • 김중배;이동희;신운섭;고춘명
    • The Korean Journal of Food And Nutrition
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    • v.11 no.3
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    • pp.347-353
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    • 1998
  • An antibiotic for methicillin resistant Staphylococcus aureus(MRSA) produced by Streptomyces lydicus YSK-681 was extracted by chloroform, and then purified by the C18 reversed-phase HPLC and silica gel column HPLC. The molecular weight of the purified antibiotic was determined from the FAB analysis MS an m/z 1022.4 and 1036.4(M+H)+, indicating that the isolated antibiotic consisted of two similar compounds with the molecular weight difference of 14 m/z value. With the aid of the various nuclear magnetic resonance(NMR) spectroscopic techniques such as 1H NMR, 13C NMR, DEPT and HMQC spectroscopy, the characteristics of function al groups were deduced as the hydroxyl group and leucine. The MIC values of the purified antibiotic were observed at 1∼32 $\mu\textrm{g}$/$m\ell$ against Gram-positive bacteria compared to > 125 $\mu\textrm{g}$/$m\ell$ against Gram-negative bacteria or fungi. The antibiotic was active at 8 $\mu\textrm{g}$/$m\ell$ of MIC90 and S180 at the concentration of 500 $\mu\textrm{g}$/$m\ell$.

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Diarylheptanoids from Bark of Alnus hirsuta Turcz (물오리나무 수피의 Diarylheptanoid)

  • Hwang, Byung-Ho;Cho, Jae-Hyun;Lee, Tae-Seong;Bae, Young-Soo
    • Journal of the Korean Wood Science and Technology
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    • v.37 no.1
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    • pp.73-77
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    • 2009
  • This study was carried out to investigate the valuable antioxidative compound from extracts of Alnus hirsuta Turcz. which has a nationwide distribution. The bark (2 kg) was extracted with 70% aqueous acetone and fractionated, and the ethyl acetate and $H_2O$ fractions, separately, were chromatographed on a Sephadex LH-20 column to purify the mixture and to give two diarylheptanoid compounds. The isolated compounds were analyzed by NMR spectroscopy, including $^1H$, $^{13}C$ and two-dimensional NMR, and identified as oregonin (1) and 1,7-bis-(3,4-dihydroxyphenyl)-heptane-5-O-${\beta}$-D-xylopyranoside (2). The antioxidative activity was evaluated by DPPH method using two diarylheptanoids and acid-hydrolyzed oregonin derivative which indicated higher activity potential. Of those the acid-hydrolyzed oregonin derivative showed highly active potential with the value of 2.6 of $IC_{50}$.

Synthesis and Supramolecular Assembly of Ru(II)-Terpyridine Complexes linked with β-Cyclodextrin or Adamantyl Group (β-CD 또는 아다만탄이 결합된 루테늄(II)-터피리딘 착화합물의 제조와 초분자 조립)

  • Park, Dae-Rim;Chung, Yong-Chae;Choi, Kyung-Ho;Kim, Hyung-Jin
    • Journal of the Korean Chemical Society
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    • v.51 no.6
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    • pp.526-535
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    • 2007
  • Ru(II)-terpyridine complexes (8, 9, 11) linked with adamantyl or β-cyclodextrin moieties were synthesized and characterized based on their 1H and 13C NMR spectra as well as MS spectra. Ru(II)-terpyridine complexes (8, 11) linked with adamantyl moiety were readily dissolved in aqueous solution via encapsulation by β-cyclodextrin when they were mixed with an equimolar amount of β-cyclodextrin. In the similar way, the adamantane guest of the Ru(II)-terpyridine complexes (8, 11) were encapsulated by β-cyclodextrin moiety of the ruthenium complex 9 to afford supramolecular assemblies in aqueous environment. Formation of assemblies was corroborated by 1H NMR spectroscopy.

Isoprene/n-pentane separation using facilitated transport membranes with SPEEK-AgNO3 (SPEEK-AgNO3로 이루어진 촉진 수송 분리 막을 사용한 isoprene/n-pentane 혼합물 분리)

  • Choi, Hyun Woo;Kim, Dong Bum;Kim, Hoon Sik;Lee, Chang Ha;Choi, Dae Ki
    • Clean Technology
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    • v.10 no.3
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    • pp.169-176
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    • 2004
  • Sulfonated ionomer membranes, sulfonated poly(ether ether)ketone (SPEEK)-$AgNO_3$, were prepared and tested for separation of the isoprene/n-pentane mixtures. The facilitated transport membranes showed good selectivity and permeance of isoprene over n-pentane and long-term stability. Depending on various reaction conditions, the degree of sulfonation (DS) of SPEEK was measured by 1H NMR spectroscopy and the performance of the membranes was affected by the DS of SPEEK as a whole. As the DS of SPEEK was increased, the selectivity of isoprene over n-pentane increased and eventually reached a maximum selectivity of 850 ~ 900 and the stability of that was continued more than 100 h.

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Photoreactivity of $ReH_5$(Cyttp) (Cyttp=Php$(CH_2CH_2CH_2PCy_2)_2)$ with CO, $CO_2\;and\;PMe_3$

  • Lee, Myung-Young;Shin, Dae-Ho;Kim, You-Hyuk
    • Bulletin of the Korean Chemical Society
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    • v.15 no.7
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    • pp.571-576
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    • 1994
  • The photoreactions of $ReH_5(Cyttp)\;(1)\;(Cyttp=PhP(CH_2CH_2CH_2PCy_2)_2)\;with\;CO,\;CO_2\;and\;PMe_3 has been investigated to find the differences in reactivities from those of trismonophosphine analog. Irradiation of 1 under CO, $CO_2$ and excess $PMe_3$ in benzene results in the formation of the complexes, $ReH(CO)_2(Cyttp)\;(2),\;ReH_2({\eta}^2-HCO_2)(Cyttp)\;(3)\;and\;$ReH_3(PMe_3)(Cyttp)$ (4), respectively. The resulting products suggest that photoreactions of $ReH_5(Cyttp)$ proceed by photoextrusion of $H_2$ giving a phototransient species "$ReH_3$(Cyttp)" which can be trapped by CO, $CO_2\;and\;PMe_3$. The structures of 2, 3 and 4 are inferred based on $^1H,\;^{31}P$ NMR and I. R spectroscopy.

Research fecal metabolite according to fed different ratios of roughage to concentrate on lactating cow using 1H-NMR analysis (조사료와 농후사료 급여비율에 따른 젖소 우분의 대사체 탐색)

  • Kim, Hyun Sang;Lee, Shin Ja;Eom, Jun Sik;Lee, Sung Sill
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.21 no.2
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    • pp.432-439
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    • 2020
  • This study examined the metabolites in different roughage to concentrate ratios using proton nuclear magnetic resonance spectroscopy (1H-NMR). Six lactating cows were divided into two groups that were fed different roughage to concentrate ratios (HR group = 8:2, HC group = 2:8). Feces samples were collected individually at one time, and the metabolites were analyzed using an SPE-800 MHz NMR-MS system. The metabolites were identified and quantified using a Chenomx NMR suite 8.4. Metabolic pathway analysis and principal component analysis were conducted using a Metaboanalyst 4.0. Statistical analysis was performed using a Dunnett's test on the SAS program. As a result, several metabolites were identified, and among them, 77 metabolites were used in statistical analysis. The levels of twelve metabolites were significantly higher in the HC group: succinate, dimethylamine, histamine, homovanillate, thymol, acetate, propionate, butyrate, isovalerate, valerate, imidazole, N-nitrosodimethylamine, and O-acetylcholine. In the HC group, the concentrations of all metabolites were higher than in the HR group, and the metabolic pathway was also different. This study is expected to be useful for a variety of livestock studies by 1H-NMR because it examined the change in metabolites in the body metabolism and microorganisms.

Effect of Crown Ring Size and Upper Moiety on the Extraction of s-Block Metals by Ionizable Calixcrown Nano-baskets

  • Mokhtari, Bahram;Pourabdollah, Kobra
    • Bulletin of the Korean Chemical Society
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    • v.32 no.11
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    • pp.3979-3990
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    • 2011
  • Eight ionizable nano-baskets of cone 25,26-di(carboxymethoxy)calix[4]arene-crown-3,4,5,6 were synthesized and were verified by $^1H$ and $^{13}C$ NMR spectroscopy, IR spectroscopy and elemental analysis. The competitive solvent extractions of alkali and alkaline earth metal cations were studied using such nano-baskets. The novelty of this study is including three binding units of calixarene's bowl, crown ether's ring and electron-donor ionizable moieties in a unique scaffold to assess the binding tendency towards the cations. The objective of this work is to study the extraction efficiency, selectivity and $pH_{1/2}$ of such complexes. The result of solvent extraction experiments indicated that these compounds were effective extractants of alkali and alkaline earth metal cations. Their selectivities were greatly influenced by the acidity of solution and the conformations of the calixcrown. One conformer was selective to $Na^+$ in pH ${\geq}$ 4, while the other was highly selective to $Ba^{2+}$ in pH 6 and upper.

Characterization of a thermostable fructosyltransferase from Leuconostoc mesenteroides TL1

  • Lee, Gwang-Ok;Gang, Hui-Gyeong;Kim, Do-Man
    • 한국생물공학회:학술대회논문집
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    • 2003.04a
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    • pp.527-529
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    • 2003
  • A fructosyltransferase from Leuconostoc mesenteroides TL1 was purified. The molecular mass of the enzyme was estimated to be 38 kDa based on the activity staining. The pH and temperature optima of the enzyme were 6.3 and $40^{\circ}C$, respectivly. Structural analysis of the polymer prepared from sucrose by the enzyme was determined by NMR Spectroscopy: It shows the heterogeneous linkages of levan-like fructan and dextran-like glucan.

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