• Title/Summary/Keyword: NMR and Mass Spectra

Search Result 97, Processing Time 0.027 seconds

Extractives from Epimedium koreanum Nakai (삼지구엽초(Epimedium koreanum Nakai)의 추출성분)

  • Lee, Tae-Seong;Cho, Jae-Hyun;Hwang, Byung-Ho
    • Journal of Korea Foresty Energy
    • /
    • v.24 no.2
    • /
    • pp.16-23
    • /
    • 2005
  • The air dried of Epimedium koreanum Nakai was extracted with MeOH and its extractives were concentrated with a vacuum evaporator. The extractives were fractionated with a series of n-hexane, chloroform (${CHCl}_3$), butanol (BuOH), ethyl acetate (EtOAc) and water on a separately funnel. Each fraction was freeze dried to give some dark brown powder. The EtOAc and BuOH soluble fractions were chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-n-hexane mixture as eluents. The isolated compounds were tested with a cellulose TLC developed with TBA and 6% acetic acid and then visualized on UV lamp or sprayed with vanillin-HCl-EtOH. The purified compounds were flavonoids and their glycosides, and organic acid as follows : (+)-catechin, icariin, hyperoside, Ikarisoside A and caffeic acid. The structures of each compounds were confirmed by $^1H-NMR,\;^{13}C-NMR$ and Mass spectra. Also, executed qualitative analysis as use GC/MS(Libraries search) about ${CHCl}_3$ soluble compounds of each part.

  • PDF

Synthesis and Characterization of Low Viscosity Aromatic Hyperbranched Polyester Epoxy Resin

  • Zhang, Daohong;Jia, Demin;Zhou, Zihu
    • Macromolecular Research
    • /
    • v.17 no.5
    • /
    • pp.289-295
    • /
    • 2009
  • Low viscosity aromatic hyperbranched polyester epoxy resin (HTBE) was synthesized by the reaction between epichlorohydrin (ECH) and carboxyl-end hyperbranched polyester (HTB) which was prepared from inexpensive materials $A_2$ (1,4-butanediol glycol, BEG) and $B_3$ (trimellitic anhydride, TMA) by pseudo one-step method. The molar mass of the HTB was calculated from its acid value by "Recursive Probability Approach". The degree of branching (DB) of the HTB was characterized by model compounds and $^1H$ NMR-minus spectrum technology, and the DB of the HTB was about $0.47{\sim}0.63$. The viscosity and epoxy equivalent weight of the HTBE were $3,600{\sim}5,000\;cp$ and lower than 540 g/mol respectively. The reaction mechanism and structure of the $AB_2$ monomer, HTB and HTBE were investigated by MS, $^1H$ NMR and FTIR spectra technology. The molecular size of HTBE is under 8.65 nm and its shape is ellipsoid-like as determined by molecular simulation.

Inhibitory Activity against Helicobacter pylori of Isolated Compounds from Pinus koraiensis Siebold et Zucc Leaves

  • Jo, Bun-Sung;Cho, Young-Je
    • Journal of Applied Biological Chemistry
    • /
    • v.59 no.1
    • /
    • pp.19-23
    • /
    • 2016
  • A phenol substance was extracted from Pinus koraiensis Siebold et Zucc leaf extracts and its biological efficacy was measured. The highest content of the phenol substance contained in Pinus koraiensis Siebold et Zucc leaves was 13.5 mg/g, which was obtained when it was extracted with 80% ethanol. At a concentration of 200 mg/mL, the phenolic substances extracted with 80% ethanol and water showed antimicrobial activities against Helicobacter pylori, producing clear zones of 10 and 12 mm diameter, respectively. Pinus koraiensis Siebold et Zucc. leaf extracts were separated using a Sephadex LH-20 column and 4 fractions were obtained (fractions A-D). Fractions C and D showed the greatest inhibitory activity against Helicobacter pylori producing 10.1 and 12.3 mm clear zones, respectively. These two fractions were purified using a Sephadex LH-20 and MCI-gel column ($H_2O{\rightarrow}100%$ ethanol). Purified compounds A and B were identified as syringic acid and compound C was identified as p-coumaric acid based on $^1H$-nuclear magnetic resonance (NMR), $^{13}C$-NMR, and fast atom bombardment mass spectrometry spectra. When two or more purified compounds were mixed, a synergistic effect of anti-Helicobacter pylori activity was evident. This result indicates that extracts of Pinus koraiensis Siebold et Zucc leaves could be considered a functional food because of their high antimicrobial properties.

Photoresponsive Arylether Dendrimers with Azobenzene Core and Terminal Vinyl Groups

  • Lee, Ji-Hye;Choi, Dae-Ock;Park, Ji-Eun;Shin, Eun-Ju
    • Bulletin of the Korean Chemical Society
    • /
    • v.29 no.4
    • /
    • pp.761-766
    • /
    • 2008
  • Photoresponsive arylether dendrimers Bis-azo-Gn(3,5) 1a-1c and Bis-azo-Gn(3,4,5) 2a-2c (n = 1-3) with an azobenzene unit at the core and several vinyl groups (3,5-bis(but-3-enyloxy)phenyl groups or 3,4,5-tris(but-3- enyloxy)phenyl groups) at the periphery have been prepared. Their structures and reversible trans-cis isomerization behaviors have been investigated by $^1H$-NMR, $^{13}C$-NMR, MALDI-TOF-Mass, and UV-vis spectra. All six azobenzene-cored dendrimers carried out very fast trans $\rightarrow$ cis photoisomerization on irradiation of 350 nm light and reached to the photostationary state within 180 s. During the dark incubation, slow thermal back reversion from cis to trans form is observed for all six dendrimers and is completed within 3 days for 1a-1c and 1 day for 2a-2c. Isomerization efficiency decreases with increasing generation. However, the initial reaction rates of both trans $\rightarrow$ cis photochemical isomerization and cis $\rightarrow$ trans thermal isomerization increases significantly with increasing generation for dendrimers for 1a-1c but only slightly for 2a-2c.

Characterization and Structural Determination of the Antibiotics Produced by a Clostridium sp. KH-431 (Clostridium sp. KH-431이 생산하는 항생물질의 특성 및 구조)

  • 홍수형;김경석;박용복;하지홍;이재근
    • Microbiology and Biotechnology Letters
    • /
    • v.21 no.1
    • /
    • pp.47-53
    • /
    • 1993
  • Antibiotics KG-431A and KG-431B were isolated from the fermentation broth of the Clostridium sp. KH-431. As we have shown previously, only KG-431B was successful to recrystallize. These antibiotics showed antimicrobial activities against broad spectrum of bacteria and fungi. KG-431B also showed anticancer activity against some animal tumor cells according to the SRB method. Physico-chemical properties of KG-431B were determined using UV, IR, NMR and Mass spectra. It was identified to be 3-Indole propionic acid and the structure of the KG-431A is currently under investigation.

  • PDF

Synthesis and Characterization of Molybdenum Complexes with Schiff Bases (I). Bis-(N-aryl salicylaldiminato) of dioxomolybdenum (VI) Complexes (몰리브덴의 시프-염기착물의 합성과 그 성질 (제1보). 다이옥소 몰리브데늄(VI)의 아릴살릴실알디미나토착물)

  • Oh Sang Oh;Bon Kweon Koo
    • Journal of the Korean Chemical Society
    • /
    • v.29 no.3
    • /
    • pp.226-232
    • /
    • 1985
  • Dioxomolybdenum(VI) complexes, MoO$_2$(H-Sal-R)$_2$, R; arylamines, have been synthesized by reactions of dioxobis (salicylaldehydato) molybdenum(VI) with various primary amines. These complexes have been characterized by electric conductivity and spectroscopic studies. Infrared, uv-vis, and proton nmr spectra show that the complexes are six-coordinated with cis-MoO$_2$ group. And mass spectra indicates that the combining ratios for Mo (VI)-ligand are 1 : 2. They are yellow, stable for a considerably long time in the atmosphere at room temperature and slightly soluble in alcohol, dichloromethane and dimethylformamide but insoluble in benzene, ether and carbon tetrachloride.

  • PDF

Synthesis and Structure of Nickel(II) Complex with N-Benzylisonitrosoacetylacetone Imine (N-Benzylisonitrosoacetylacetone Imine Ni(II) 착물의 합성 및 구조)

  • Byung Kyo Lee;Dae Sub O;Heung Lark Lee
    • Journal of the Korean Chemical Society
    • /
    • v.32 no.6
    • /
    • pp.536-542
    • /
    • 1988
  • A nickel(Ⅱ) complex, Ni(IAA-NBz) (IAA-NBz') with ligand, N-benzylisonitrosoacetyl acetone imine (H-IAA-NBz) has been synthesized. This complex is very stable at room temperature and has cis-form and trans-form isomers. The ratio of nickel (Ⅱ) ion and ligand combined is 1 : 2. The elemental analysis, ir, nmr. electronic spectra and mass spectra have been studied. It is suggested from these studies that the isonitroso group of one ligand, H-IAA-NBz coordinates to nickel(Ⅱ)ion through the nitrogen atom to form five-membered ring, while that of the other ligand, H-IAA-NBz coordinates to nickel (Ⅱ) ion through the oxygen atom to form six-membered ring in square-planar complex.

  • PDF

A Tumor Growth Inhibitory Substance Isolated from Panax ginseng (고려홍삼분말중의 항종양 활성물질)

  • Katano Mitsuo;Yamamoto Hiroshi;Matsunaga Hisashi
    • Proceedings of the Ginseng society Conference
    • /
    • 1988.08a
    • /
    • pp.33-35
    • /
    • 1988
  • During a series of studies aimed at isolation of the tumor growth inhibitory substance from Panax ginseng. we found a new type of antitumor substance. The substance was isolated from a powder of the root of Panax ginseng C.A. Meyer. which is commonly used for various diseases as a commercial medical drug by the name of Korean Red Ginseng Powder in Japan. Data from infrared spectra proton and carbon-13 nuclear magnetic resonance. and high resolution mass spectra were identical with those of panaxytriol. Panaxytriol isolated from Korean Red Ginseng Powder (Nikkan Korai Ninjin Co.. Ltd.. Japan) inhibited the growth of several kinds of human and murine malignant cells in vitro. Although the detailed mechanism of cell growth inhibition by panaxytriol is yet to he elucidated. panaxytriol's action appeares to be more dose-dependent than time-dependent.

  • PDF

Isolation and Oxidation Characteristics of Alkaloids of Aconitum volubile (가는줄돌쩌기 알칼로이드 성분의 분리 및 산화적 특성)

  • Heo, Kyong-Hee;Lee, Chung-Kyu
    • Korean Journal of Pharmacognosy
    • /
    • v.39 no.2
    • /
    • pp.127-134
    • /
    • 2008
  • From the under ground part of Aconitum volubile Pall. (Ranunculaceae),seven nor- or di-terpenoid alkaloids were isolated and identified by NMR spectra and mass spectrum. The alkaloids were three $C_{19}$-norditerpenoid alkaloids such as isotalatizidine, altaconitine and vilmorrianine A, and four $C_{20}$-diterpenoid alkaloids such as 12-epidehydronapelline, 12-epinapelline, songoramine and songorine. Some of the isolated diterpenoid alkaloids were subjected to oxidation reaction with active $MnO_2$ and oxoammonium salt. The results were C-12 oxidation(ketone formation) and N-dealkylation in veatchin-type and decomposition to non-alkaloidal compounds in atisine-type ajaconine.

Studies on the Components of Evodia daniellii $H_{EMSLEY}$ in Korea (한국산 오수유성분에 관한 연구)

  • Chung, Bo-Sup
    • Korean Journal of Pharmacognosy
    • /
    • v.1 no.4
    • /
    • pp.119-124
    • /
    • 1970
  • Evodia daniellii $H_{EMSLEY}$, a plant belonging to Rutaceae, is cultivated in Korea and used as a folkmedicine for gastric inflammation, extermination of noxious insects, and headache. The seed oil of this plant also has been used in various diseases, for example, dermatitis, scabies and so forth. From the barks, fruit peels, and seed oil of Evodia daniellii $H_{EMSLEY}$, four crystalline compounds were isolated. Three compounds except one were characterized as methyl sinapate, bergapten, and evodiamine by m.p. determination, elemental analysis, UV, IR, NMR spectra and mass analysis. Even though methyl sinapate was a known synthetic compound, it was not yet reported as a natural product. From the seed oil, unsaponifiable fraction was separated and was analyzed. It was considered to be consisted with sterols, hydrocarbons and tocopherols.

  • PDF