• 제목/요약/키워드: $^1H$ NMR

검색결과 2,518건 처리시간 0.031초

Solubility Enhancement of Flavonoids by Cyclosophoraose Isolated from Rhizobium meliloti 2011

  • Kang Si-Mook;Lee Sang-Hoo;Kwon Chan-Ho;Jung Seun-Ho
    • Journal of Microbiology and Biotechnology
    • /
    • 제16권5호
    • /
    • pp.791-794
    • /
    • 2006
  • Cyclosophoraose (cyclic $\beta-(1,2)-glucan$, Cys) isolated from Rhizobium meliloti, a soil microorganism, was used as a solubility enhancer for flavonoids. The complexes of the cyclic oligosaccharide with flavonoids were confirmed through $^1H$ nuclear magnetic resonance (NMR) spectroscopic analysis. Flavonoids solubilized by Cys were quantitatively analyzed through high-performance liquid chromatography (HPLC). Among the flavonoids tested, the solubility of naringenin was greatly enhanced by Cys, compared with other compounds. The solubility of naringenin was enhanced about 7.1-fold by adding 10 mM Cys, compared with a control. $^1H$ NMR spectroscopic analysis indicated that the H-6 and H-8 protons, which are located on the A ring of naringenin, were greatly shifted upfield upon the complexation with Cys. This result suggested that Cys showed a regioselective interaction with the naringenin molecule upon the complexation, resulting in the solubility enhancement of naringenin.

Solid State Dynamic Nuclear Polarization of 1H Nuclear Spins at 0.3 T and 4.2 K

  • Shim, Jeong Hyun
    • 한국자기공명학회논문지
    • /
    • 제21권4호
    • /
    • pp.114-118
    • /
    • 2017
  • Here, I report solid state Dynamic Nuclear Polarization (DNP) of $^1H$ nuclear spins at 0.3 T and 4.2 K. The DNP polarizer was developed based on a commercial X-band Electron Spin Resonance (ESR) modified for DNP, in combination with a NMR console and a liquid-Helium cryostat. By detuning magnetic field, DNP spectrum was measured to find the optimal condition. At +3 mT detuned from on-resonance field, $^1H$ NMR signal of 60:40 glycerol/water frozen solution doped with 20 mM perdeuterated-Tempone was amplified 43 times. The $^1H$ spin polarization obtained at 4.2 K is over 3100 times higher than that at 300 K. The width of the DNP spectrum, which is five times broader than ESR spectrum, is inconsistent with solid effect or thermal mixing, and presumably suggests a different DNP mechanism.

Diffusional Behavior of Rodlike Poly(${\gamma}-benzyl$ L-glutamate) in Concentrated Solution as Studied by the Field-Gradient $^{1}H$ NMR Methods

  • Kuroki, Shigeki
    • 한국고분자학회:학술대회논문집
    • /
    • 한국고분자학회 2006년도 IUPAC International Symposium on Advanced Polymers for Emerging Technologies
    • /
    • pp.345-345
    • /
    • 2006
  • It is well known that poly(glutamate)s with long n-alkyl side chains form thermotropic liquid crystalline state by melting of the side-chain crystallites and also poly(glutamate)s such as poly(${\gamma}-benzyl\;L-glutamate$ )(PBLG), poly(${\gamma}-n-alkyl\;L-glutamate$), etc. in solvent form the isotropic, biphasic and liquid crystalline phases which contains cholesteric and columnar liquid crystalline forms depending on the polypeptide concentration. Although there is no diffusion study for PBLG in liquid crystalline state, because it is difficult to observed $^{1}H$ spectrum of PBLG in liquid crystalline state for its very short $^{1}H\;T_{2}$. In this study, the diffusional behavior of rodlike PBLG in concentrated solution is successfully elucidated as studied by the field-gradient $^{1}H$ NMR methods.

  • PDF

조릿대잎의 flavone 배당체 성분 (The flavone glycosides of Sasa borealis)

  • 윤기동;김철영;허훈
    • 생약학회지
    • /
    • 제31권2호
    • /
    • pp.224-227
    • /
    • 2000
  • As part of study of the constituents of bamboo grasses, the leaves of Sasa borealis (Hackel) Makino (Gramineae) were examined. Friedelin, glutinol, isoorientin and isovitexin have been reported as constituents of bamboo grasses. In this study, tricin and two flavone glycosides, tricin $7-O-{\beta}-D-glucopyranoside$ and luteolin $6-C-{\alpha}-L-arabinopyranoside$ have been isolated from EtOAc extract of S. borealis, by consecutive silica gel, Sephadex LH-20 column chromatography and a repetitive HPLC. The structures of these compounds were determined by IR, $^1H-NMR,\;^{13}C-NMR,\;^{13}C-^1H\;COSY,\;^1H-^1H\;COSY,\;HMBC$ and Mass spectral data.

  • PDF

Isolation of Handelin from Chrysanthemum boreale

  • Kang, Sam-Sik;Kim, Ju-Sun;Son, Kun-Ho;Lee, Chong-Ock;Kim, Young-Hee
    • Archives of Pharmacal Research
    • /
    • 제19권5호
    • /
    • pp.406-410
    • /
    • 1996
  • The flowers of Chrysanthemum boreale afforded handelin, a unique guaianolide dimer and a mixture of n-hydrocarbons and n-hydrocarbon alcohols in addition to b-sitosterol and b-sitosterol glucoside. Detailed analysis of the $^{1}H$- and $^{13}C$-NMR spectra of handelin was carried out by the application of two-dimensional $^{1}H-^{1}H$-COSY and $^{1}H$- $^{13}C$ multiple-bond, multiple-quantum spectroscopic correlation techniques. Handelin was inactive in the in vitro anti-tumor activity.

  • PDF

¹H NMR Study of the Inclusion Complexes of Chiral Aromatic Guests with β-Cyclodextrin and Its Derivatives: Discrimination of Aromatic Protons and Chiral Recognition

  • 고광희;박종목
    • Bulletin of the Korean Chemical Society
    • /
    • 제17권11호
    • /
    • pp.1052-1056
    • /
    • 1996
  • The effects of β-CD, Me-β-CD, and biphenyl capped β-CD on 1H NMR spectra of mandelic acid 1, α-methylbenzylamine 2 and 2-phenylpropionic acid 3 were investigated. Enantiomeric recognition was observed for mandelic acid 1 by all the hosts used, for α-methylbenzylamine 2 by β-CD and Me-β-CD, and for 2-phenylpropionic acid 3 by Me-β-CD. In the presence of biphenyl-capped β-CD, ο-, m-, and p-protons of the phenyl groups of the guests are discriminated due to ring current of the capped biphenyl group. The splitting pattern of the phenyl protons indicates that the phenyl group of the guests is inserted into the β-CD cavity from the secondary hydroxyl side and positioned in close proximity to the capped biphenyl ring. The magnitude of the upfield shifts of H3 and H5 protons of β-CD upon binding of guests 1-3 is similar to that caused by ephedrine or pseudoephedrine, suggesting that the substitution at benzylic carbon atom has little effect on the depth of the insertion of the phenyl group into the β-CD cavity and stability of the inclusion complexes.

Low Cost and Portable Parahydrogen Generator for the PHIP

  • Kwon, Soonmo;Min, Sein;Chae, Heelim;Namgoong, Sung Keon;Jeong, Keunhong
    • 한국자기공명학회논문지
    • /
    • 제21권4호
    • /
    • pp.126-130
    • /
    • 2017
  • In the developed NMR hyperpolarization techniques, Parahydrogen-Induced Polarization (PHIP) technique is widely utilized to overcome the low sensitivity of the NMR/MRI. Parahydrogen generator is essential to produce high spin order of parahydrogen molecule. Commercial parahydrogen generator is well developed with user-friendly systems. However, it has drawbacks of long preparation time (~ 2h including cooling down time of 1h) and high cost (~ 200 million won) for the commercial setup. We designed a simple and portable parahydrogen generating system with low cost (~ 2 million won), which produce polarization in less than 1 min. With the designed parahydrogen generator, we successfully performed the PHIP with Wilkinson's catalyst on styrene. This study will broaden the parahydrogen based polarization transfer study on many researchers by providing the simple portable and low cost parahydrogen generator.

Synthesis of Dendrimer Based Polymeric and Macrocyclic Complexes with a Platinum-Acetylide ${\pi}-Conjugated$ Organometallic Core

  • Jang, Woo-Dong
    • Macromolecular Research
    • /
    • 제13권4호
    • /
    • pp.334-338
    • /
    • 2005
  • A three-layered poly(benzyl ether) dendrimer having a bis-ethynylbenzene core was synthesized and characterized with $^{1}H$ NMR and MALDI-TOF-MS spectroscopy. The dendrimer was reacted with platinum complexes to obtain platinum-acetylide based organometallic polymers. When the dendrimer was reacted with trans-[$PtCl_{2}(PEt_{3})_{2}$], a high molecular weight polymeric compound was formed, whereas, with cis-[$PtCl_{2}dppp$], a uniform molecular weight compound was formed, which was found to be a dimeric metallacycle by $^{1}H\;NMR,\;^{31}P\;NMR$ and ESI-TOF-MS spectroscopy. Both these complexes exhibited relatively a strong emission around 440 nm, indicating that they could be potential candidates for blue emitting polymer LEDs.

폐수처리 슬럿지와 퇴비 및 목탄의 화학적 특성과 구조에 관한 연구 (A Study on the Chemical Composition and Structure of Sludge, Compost and Charcoal)

  • 임기표;위승곤
    • 펄프종이기술
    • /
    • 제35권1호
    • /
    • pp.27-32
    • /
    • 2003
  • To understand the chemical structure of sewer sludge in comparison with commercial compost and charcoal used as a soil improver, it was carried out to analyse their ash contents and metal ions, and to elucidate the chemical structure of their residuals after a sequential treatment of alcohol-benzene(1:2) extraction in Soxhlet, 3% HCl reflux and 79% H₂SO₄ hydrolysis, using CHNS analyzer and solid C-13 NMR spectrometer. The results obtained were as follows: 1. Ash content of sludge was about 46% that is higher than those of compost (17%) and charcoal (4%). 2. The residual of sludge after a sequential treatment of HCl and H₂SO₄ hydrolyses had high ash content about 23%, too. 3. The sludge seems to be suitable to the soil improver because the content of heavy metal ions in sludge was near the compost and below the organic fertilizer standard. 4. Elemental composition of sludge residual after HCl-H₂SO₄ hydrolyes was C/sub 56/H/sub 91/O/sub 12/N₂S = (C/sub 6/H/sub 10/O/sub 5/)/sub 7/(C/sub 6/H₄)/sub 7/C₂H/sub 43/O₂N₂S, similar to C/sub 103/H/sub 122/O/sub 33/N/sub 6/S = (C/sub 6/H/sub 10/O/sub 5/)/sub 6/(C/sub 6/H₄)/sub 10/C/sub 7/H/sub 22/O₃N/sub 6/S of compost. 5. The sludge residual had proved to have both considerable aliphatic and aromatic groups, but the compost residual to have mainly aliphatic groups and the charcoal to have mainly aromatic groups, through the peak analysis of solid C-13 NMR charts. 6. So, the sewer sludge is proved to have a considerable amount of aromaticity like in woody biomass containing lignin.

A New Steroidal Glycoside from Allium macrostemon Bunge

  • Kim, Yun Sik;Cha, Joon Min;Kim, Dong Hyun;Lee, Tae Hyun;Lee, Kang Ro
    • Natural Product Sciences
    • /
    • 제24권1호
    • /
    • pp.54-58
    • /
    • 2018
  • A phytochemical investigation of Allium macrostemon Bunge (Liliaceae) afforded the new pregnane steroidal glycoside, named allimacroside F (1), along with three known glycosides, benzyl-O-${\alpha}-{\text\tiny{L}}$-rhamnopyranosyl-($1{\rightarrow}6$)-${\beta}-{\text\tiny{D}}$-glucopyranoside (2), phenylethyl-O-${\alpha}-{\text\tiny{L}}$-rhamnopyranosyl-($1{\rightarrow}6$)-${\beta}-{\text\tiny{D}}$-glucopyranoside (3), (Z)-3-hexenyl-O-${\alpha}-{\text\tiny{L}}$-rhamnopyranosyl-($1{\rightarrow}6$)-${\beta}-{\text\tiny{D}}$-glucopyranoside (4). The identification and structural elucidation of a new compound (1) was carried out based on spectral data analyses ($^1H-NMR$, $^{13}C-NMR$, $^1H-^1H$ COSY, HSQC, HMBC, and NOESY) and HR-FAB-MS.