• Title/Summary/Keyword: }NMR$

Search Result 4,971, Processing Time 0.042 seconds

Structure and Hydrolysis Study of Inclusion Complex of Cyclodextrin and Aspirin (시클로덱스트린과 아스피린의 포접화합물의 구조와 가수분해에 관한 연구)

  • 최희숙;김경순
    • Journal of Life Science
    • /
    • v.10 no.1
    • /
    • pp.86-93
    • /
    • 2000
  • Specific molecular recognition of cyclodextrin and aspirin was determined. A stable 1:1 inclusion complex was established in solution. The distinct structure of inclusion complex was elucidated by FT-IR, FAB-MS, UV, 1H NMR, and 13C NMR spectroscopy. Based on the 1H NMR data, a time-averaged conformation of $\alpha$-cyclodextrin exhibited significant catalytic activity toward the hydrolysis of aspirin in alkaline solution.

  • PDF

Application of Deuterium NMR Analysis for the Differentiation of Korean and Foreign Liquors (중수소 핵자기 공명을 이용한 외국 술과 국산 술의 비교 분석)

  • Han, Gee-Chung;Lee, Sueg-Geun
    • Analytical Science and Technology
    • /
    • v.13 no.1
    • /
    • pp.127-129
    • /
    • 2000
  • The $^2H$ NMR analysis was used to determine the relative deuterium contents at the position of methyl and methylene in ethyl alcohols. Four different liquors manufactured in Korea clearly showed different R values from those of foreign liquors. These R values for the Korean liquors could be used to distinguish adulteration.

  • PDF

NMR study on secondary metabolites isolated from an identified tunicate

  • Rho, Jung-Rae
    • Journal of the Korean Magnetic Resonance Society
    • /
    • v.8 no.2
    • /
    • pp.115-126
    • /
    • 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.

  • PDF

In Vivo $^{13}C$-NMR Spectroscopic Study of Polyhydroxyalkanoic Acid Degradation Kinetics in Bacteria

  • Oh, Jung-Sook;Choi, Mun-Hwan;Yoon, Sung-Chul
    • Journal of Microbiology and Biotechnology
    • /
    • v.15 no.6
    • /
    • pp.1330-1336
    • /
    • 2005
  • Polyhydroxyalkanoic acid (PHA) inclusion bodies were analyzed in situ by $^{13}C$-nuclear magnetic resonance ($^{13}C$-NMR) spectroscopy. The PHA inclusion bodies studied were composed of poly(3-hydroxybutyrate) or poly(3hydroxybutyrate-co-4-hydroxybutyrate), which was accumulated in Hydrogenophaga pseudoflava, and medium-chain-length PHA (MCL-PHA), which was accumulated in Pseudomonas fluorescens BM07 from octanoic acid or 11-phenoxyundecanoic acid (11-POU). The quantification of the $^{13}C$-NMR signals was conducted against a standard compound, sodium 2,2-dimethyl-2-silapentane-5-sulfonate (DSS). The chemical shift values for the in vivo NMR spectral peaks agreed well with those for the corresponding purified PHA polymers. The intracellular degradation of the PHA inclusions by intracellular PHA depolymerase(s) was monitored by in vivo NMR spectroscopy and analyzed in terms of first-order reaction kinetics. The H. pseudoflava cells were washed for the degradation experiment, transferred to a degradation medium without a carbon source, but containing 1.0 g/l ammonium sulfate, and cultivated at $35^{\circ}C$ for 72 h. The in vivo NMR spectra were obtained at $70^{\circ}C$ for the short-chain-length PHA cells whereas the spectra for the aliphatic and aromatic MCL-PHA cells were obtained at $50^{\circ}C\;and\;80^{\circ}C$, respectively. For the H. pseudoflava cells, the in vivo NMR kinetics analysis of the PHA degradation resulted in a first-order degradation rate constant of 0.075/h ($r^{2}$=0.94) for the initial 24 h of degradation, which was close to the 0.050/h determined when using a gas chromatographic analysis of chloroform extracts of sulfuric acid/methanol reaction mixtures of dried whole cells. Accordingly, it is suggested that in vivo $^{13}C$-NMR spectroscopy is an important tool for studying intracellular PHA degradation in terms of kinetics.

Detection of Iron Nanoparticles using Nuclear Magnetic Resonance Relaxometry and Inverse Laplace Transform

  • Kim, Seong Min
    • Journal of Biosystems Engineering
    • /
    • v.39 no.4
    • /
    • pp.345-351
    • /
    • 2014
  • Purpose: Rapid detection of bacteria is very important in agricultural and food industries to prevent many foodborne illnesses. The objective of this study was to develop a portable nuclear magnetic resonance (NMR)-based system to detect foodborne pathogens (E. coli). This study was focused on developing a method to detect low concentrations of magnetic nanoparticles using NMR techniques. Methods: NMR relaxometry was performed to examine the NMR properties of iron nanoparticle mixtures with different concentrations by using a 1 T permanent magnet magnetic resonance imaging system. Exponential curve fitting (ECF) and inverse Laplace transform (ILT) methods were used to estimate the NMR relaxation time constants, $T_1$ and $T_2$, of guar gum solutions with different iron nanoparticle concentrations (0, $10^{-3}$, $10^{-4}$, $10^{-5}$, $10^{-6}$, and $10^{-7}M$). Results: The ECF and ILT methods did not show much difference in these values. Analysis of the NMR relaxation data showed that the ILT method is comparable to the classical ECF method and is more sensitive to the presence of iron nanoparticles. This study also showed that the spin-spin relaxation time constants acquired by a Carr-Purcell-Meiboom-Gill (CPMG) pulse sequence are more useful for determining the concentration of iron nanoparticle solutions comparwith the spin-lattice relaxation time constants acquired by an inversion recovery pulse sequence. Conclusions: We conclude that NMR relaxometry that utilizes CPMG pulse sequence and ILT analysis is more suitable for detecting foodborne pathogens bound to magnetic nanoparticles in agricultural and food products than using inversion recovery pulse sequence and ECF analysis.

The Laccase Activity of Trametes versicolor during Cultivation on Acetylated Wood and 13C-CP/MAS NMR Study (아세틸화 처리 목재에 배양시킨 Trametes versicolor의 Laccase활성과 13C-CP/MAS NMR 분석)

  • Son, Dong-Won;Lee, Dong-Heub
    • Journal of the Korean Wood Science and Technology
    • /
    • v.29 no.4
    • /
    • pp.60-66
    • /
    • 2001
  • For examine anti-degradation factors of acetylated wood, acetylated wood was incubated on Trametes versicolor. The laccase activity was examined in broth culture and solid fermentation that contain acetylated chips. The change of acetyl groups and chemical composition in the acetylated wood having massloss analysed by $^{13}C$-CP/MAS NMR. The laccase activity was detected in broth culture. When the T. versicolor contact to acetylated wood directly, the laccase activity was very low and couldn't maintain during test periods. Through the analysing of $^{13}C$-CP/MAS NMR, the acetylation took place carbohydrates as well as lignin and hydroxyl group of amorphous region was more easily substituted that of crystalline region The spectral analyses of $^{13}C$-CP/MAS NMR were shown that introduced acetyl bond was stable against fungal attack.

  • PDF

Preparation and characterization of immobilized 8-hydroxyquinoline for chromatographic application (크로마토그래피용 고정화 8-hydroxyquinoline의 제조 및 특성분석)

  • Kim, Bum-Soo
    • Analytical Science and Technology
    • /
    • v.13 no.1
    • /
    • pp.49-54
    • /
    • 2000
  • The 8-hydroxyquinoline derivative of silica gel has been prepared through the 5 step reaction. We carried out infrared as well as nuclear magnetic resonance spectrometric characterization of products taken from each step of reaction. IR study of bare silica gel showed free and hydrogen bonded hydroxyl. From the 1st step reaction, we observed IR bands for N-H and C-H as well as NMR peaks for three methylene carbons in APTS group. From the 2nd step, we observed IR bands for carbonyl, nitro and aromatic carbon group with NMR peaks for aliphatic, aromatic and carbonyl carbons. The reduction of $NO_2$ group to $NH_2$ group is confirmed by IR and NMR from 3rd step reaction. In the last step, the immobilization of 8-quinolinol is confirmed by disappearance of $N{\equiv}N$ IR peak observed in 4th step.

  • PDF

INTRINSIC NMR ISOTOPE SHIFTS OF CYCLOOCTANONE AT LOW TEMPERATURE (저온에서의 싸이클로옥타논에 대한 고유동위원소 효과)

  • Jung, Miewon
    • Analytical Science and Technology
    • /
    • v.7 no.2
    • /
    • pp.213-224
    • /
    • 1994
  • Several isotopomers of cyclooctanone were prepared by selective deuterium substitution. Intrinsic isotope effects on $^{13}C$ NMR chemical shifts of these isotopomers were investigated systematically at low temperature. These istope effects were discussed in relation to the preferred boat-chair conformation of cyclooctanone. Deuterium isotope effects on NMR chemical shifts have been known for a long time. Especially in a conformationally mobile molecule, isotope perturbation could affect NMR signals through a combination of isotope effects on equilibria and intrinsic effects. The distinction between intrinsic and nonintrinsic effects is quite difficult at ambient temperature due to involvement of both equilibrium and intrinsic isotope effects. However if equilibria between possible conformers of cyclooctanone are slowed down enough on the NMR time scale by lowering temperature, it should be possible to measure intrinsic isotope shifts from the separated signals at low temperature. $^{13}C$ NMR has been successfully utilized in the study on molecular conformation in solution when one deals with stable conformers or molecules were rapid interconversion occurs at ambient temperature. The study of dynamic processes in general requires analysis of spectra at several temperature. Anet et al. did $^1H$ NMR study of cyclooctanone at low temperature to freeze out a stable conformation, but were not able initially to deduce which conformation was stable because of the complexity of alkyl region in the $^1H$ NMR spectrum. They also reported the $^1H$ and $^{13}C$ NMR spectra of the $C_9-C_{16}$ cycloalkanones with changing temperature from $-80^{\circ}C$ to $-170^{\circ}C$, but they did not report a variable temperature $^{13}C$ NMR study of cyclooctanone. For the analysis of the intrinsic isotope effect with relation to cylooctanone conformation, $^{13}C$ NMR spectra are obtained in the present work at low temperatures (up to $-150^{\circ}C$) in order to find the chemical shifts at the temperature at which the dynamic process can be "frozen-out" on the NMR time scale and cyclooctanone can be observed as a stable conformation. Both the ring inversion and pseudorotational processes must be "frozen-out" in order to see separate resonances for all eight carbons in cyclooctanone. In contrast to $^1H$ spectra, slowing down just the ring inversion process has no apparent effects on the $^{13}C$ spectra because exchange of environments within the pairs of methylene carbons can still occur by the pseudorotational process. Several isotopomers of cyclooctanone were prepared by selective deuterium substitution (fig. 1) : complete deuterium labeling at C-2 and C-8 positions gave cyclooctanone-2, 2, 8, $8-D_4$ : complete labeling at C-2 and C-7 positions afforded the 2, 2, 7, $7-D_4$ isotopomer : di-deuteration at C-3 gave the 3, $3-D_2$ isotopomer : mono-deuteration provided cyclooctanone-2-D, 4-D and 5-D isotopomers : and partial deuteration on the C-2 and C-8 position, with a chiral and difunctional case catalyst, gave the trans-2, $8-D_2$ isotopomer. These isotopomer were investigated systematically in relation with cyclooctanone conformation and intrinsic isotope effects on $^{13}C$ NMR chemical shifts at low temperature. The determination of the intrinsic effects could help in the analysis of the more complex effects at higher temperature. For quantitative analysis of intrinsic isotope effects, the $^{13}C$ NMR spectrum has been obtained for a mixture of the labeled and unlabeled compounds because the signal separations are very small.

  • PDF