• Title/Summary/Keyword: $^1H$ nuclear magnetic resonance

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NMR Relaxometry of Water in Set Yogurt During Fermentation

  • Mok, Chul-Kyoon;Qi, Jinning;Chen, Paul;Ruan, Roger
    • Food Science and Biotechnology
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    • v.17 no.5
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    • pp.895-898
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    • 2008
  • The mobility of water in set yogurt during fermentation was studied using nuclear magnetic resonance (NMR) relaxometry. The spin-spin relaxation was analyzed using a 2-fraction model, resulting in 2 spin-spin relaxation time constants $T_{21}$ and $T_{22}$. Both $T_{21}$ and $T_{22}$ exhibited rapid changes between 2 and 4 hr of fermentation, coinciding with the drop in pH and the rise in lactic acid bacteria count. The spin-lattice relaxation time $T_1$ increased over the fermentation period. Both $T_1$ and $T_2$ showed an increase in the mobility of water upon gel formation during fermentation. Water redistribution within the gel matrix due to casein aggregation and structure forming may be responsible for the changes in mobility.

Multinuclear Solid-state NMR Investigation of Nanoporous Silica Prepared by Sol-gel Polymerization Using Sodium Silicate

  • Kim, Sun-Ha;Han, Oc-Hee;Kim, Jong-Kil;Lee, Kwang-Ho
    • Bulletin of the Korean Chemical Society
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    • v.32 no.10
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    • pp.3644-3649
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    • 2011
  • Multinuclear solid-state nuclear magnetic resonance (NMR) experiments were performed to investigate the local structure changes of nanoporous silica during hydrothermal treatment and surface modification with 3-aminopropyltriethoxysilane (3-APTES). The nanoporous silica was prepared by sol-gel polymerization using inexpensive sodium silicate as a silica precursor. Using $^1H$ magic angle spinning (MAS) NMR spectra, the hydroxyl groups, which play an important role in surface reactions, were probed. Various silicon sites such as $Q^2$, $Q^3$, $Q^4$, $T^2$, and $T^3$ were identified with $^{29}Si$ cross polarization (CP) MAS NMR spectra and quantified with $^{29}Si$ MAS NMR spectra. The results indicated that about 25% of the silica surface was modified. $^1H$ and $^{29}Si$ NMR data proved that the hydrothermal treatment induced dehydration and dehyroxylation. The $^{13}C$ CP MAS and $^1H$ MAS NMR spectra of 3-APTES attached on the surface of nanoporous silica revealed that the amines of the 3-aminopropyl groups were in the chemical state of ${NH_3}^+$ rather than $NH_2$.

Nuclear Magnetic Resonance Spectroscopic Study on Inclusion Complexation of Paracyclophane with Naphthalene Derivatives in Aqueous Solution (프로톤 핵자기공명스펙트럼 측정법에 의한 수용액중 파라시클로판과 나프탈렌 유도체들간의 포접 복합체 형성에 관한 연구)

  • Chun, In-Koo
    • Journal of Pharmaceutical Investigation
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    • v.23 no.3
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    • pp.155-163
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    • 1993
  • Inclusion complexation of 1,7,21,27-tetraaza[7.1.7.1]paracyclophane (CPM 55) with 2,7-dihydroxynaphthalene (2,7-DHN) or 1,3-dihydroxynaphthalene (1,3-DHN) in pD 1.17 $DCl-D_2O$ solution was investigated by $^1H$ nuclear magnetic resonance spectroscopy (NMR) using 4,4'-dimethylaminodiphenylmethane (ACM 11) as an acyclic analog of CPM 55. In CPM 55-naphthalene derivative complex, alkyl protons located in the cavity of CPM 55 were shown to be subjected to anisotropic shielding and protons of naphthalene moiety shifted remarkably to upfield. However, in ACM 11-naphthalene derivative systems, chemical shifts for protons of both DHN compounds were not significant. The remarkable chemical shift changes suggested that the naphthalene moiety of 2,7-DHN or 1,3-DHN was included in the hydrophobic cavity of CPM 55 in aqueous solution. From the continuous variation plots of induced chemical shifts of 2,7-DHN, it was found that 2,7-DHN was included in the cavity of CPM 55 at 1:1 molar stoichiometry. Both computer simulation of a inclusion complex and strong upfield chemical shift changes of 2,7-DHN protons supported the conformation of pseudoaxial inclusion as the presumed geometry of the host-guest complex.

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Isolation and Identification of Triterpenoids and Sterols from the Flowers of Chionanthus retusus Lindl. & Paxton (이팝나무(Chionanthus retusus Lindl. & Paxton) 꽃으로부터 Triterpenoid 및 Sterol 화합물의 분리 및 동정)

  • Jung, Jae-Woo;Seo, Kyeong-Hwa;Oh, Eun-Ji;Lee, Dae-Young;Baek, Nam-In
    • Journal of Applied Biological Chemistry
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    • v.58 no.3
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    • pp.237-240
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    • 2015
  • The flowers of Chionanthus retusus Lindl. & Paxton were extracted with 80% aqueous MeOH at room temperature. The concentrated extract was partitioned as EtOAc, n-BuOH, and $H_2O$ fractions. From the EtOAc fraction, two triterpenoids and two sterols were isolated using the repeated silica gel ($SiO_2$) and octadecyl $SiO_2$ (ODS) column chromatographies. According to the results of physico-chemical and spectroscopic data including nuclear magnetic resonance, mass spectrometry, and infrared. The chemical structures of the compounds were respectively determined as ursolic acid (1), corosolic acid (2), ${\beta}$-sitosterol (3), and daucosterol (4). All the compounds were isolated for the first time from the flowers of Chionanthus retusus Lindl. & Paxton.

Effect of Cholesterol on the Phase Change of Lipid Membranes by Antimicrobial Peptides

  • Choi, Hyungkeun;Kim, Chul
    • Bulletin of the Korean Chemical Society
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    • v.35 no.5
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    • pp.1317-1322
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    • 2014
  • Membrane disruption by an antimicrobial peptide (AMP) was investigated by measuring the $^2H$ solid-state nuclear magnetic resonance spectra of 1-palmitoyl-$d_{31}$-2-oleoyl-sn-glycero-3-phosphatidylcholine (POPC_$d_{31}$) in mixtures of POPC_$d_{31}$/cholesterol and either magainin 2 or aurein 3.3 deposited on thin cover-glass plates. The line shapes of the experimental $^2H$ solid-state nuclear magnetic resonance (SSNMR) spectra were best simulated by assuming the coexistence of a mosaic spread of bilayers containing pore structures and a fasttumbling isotropic phase or a hexagonal phase. Within a few days of incubation in a hydration chamber, an isotropic phase and a pore structure were induced by magainin 2, while in case of aurein 3.3 only an isotopic phase was induced in the presence of a bilayer phase. After an incubation period of over 100 days, alignment of the bilayers increased and the amount of the pore structure decreased in case of magainin 2. In contrast with magainin 2, aurein 3.3 induced a hexagonal phase at the peptide-to-lipid ratio of 1/20 and, interestingly, cholesterol was not found in the hexagonal phase induced by aurein 3.3. The experimental results indicate that magainin 2 is more effective in disrupting lipid bilayers containing cholesterol than aurein 3.3.

Edge Enhancement due to Diffusion Effect in Magnetic Resonance Imaging (MR 영상에서 확산현상에 의한 경계강조)

  • Hong, I.K.;Ro, Y.M.;Cho, Z.H.
    • Proceedings of the KOSOMBE Conference
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    • v.1995 no.11
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    • pp.124-127
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    • 1995
  • Due to the self-diffusion of nuclear spins, the edge of phantoms is enhanced in the magnetic resonance imaging (MRI), especially in the case of microscopy [1]. According to several published works, theory has been established that the edge enhancement is caused by the motion narrowing around bounded regions due to diffusions of nuclear spins during data acquisition. It is found, however, that the signal decreases due to the diffusion attenuation and image is distorted as edge of the image is sharpened. In this paper, we wilt investigate this signal loss during data acquisition and its effects on image, i.e., image edge enhancement due to the diffusion phenomenon. This result is new and different from the previously discussed edge enhancement due to the diffusion, namely, by motion narrowing effect or spin bouncing effect at the boundary.

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The Spin-Rotation Interaction of the Proton and the Fluorine Nucleus in the Tetrahedral Spherical Top Molecules

  • Lee, Sang-Soo;Ozier, Irving;Ramsey, N.F.
    • Nuclear Engineering and Technology
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    • v.5 no.1
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    • pp.38-43
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    • 1973
  • The spin-rotation constants of the proton and tile fluorine nucleus in C $H_4$, Si $H_4$, Ge $H_4$, C $F_4$, Si $F_4$ and Ge $F_4$ were determined experimentally by the molecular beam magnetic resonance method. From the Hamiltonian and the high field approximation, the quantized energy level is given by the following equation. W $m_{I}$ $m_{J}$=- $g_{I}$ $m_{I}$H- $g_{J}$ $m_{J}$H- $C_{av}$ $m_{I}$ $m_{J}$, where $c_{av}$ is one third of the trace of the C tensor. In the nuclear resonance experiment, the proton and the fluorine nuclear resonance curves consist of many unresolved lines given by v=- $g_{J}$H- $C_{av}$ $m_{I}$, and a Gaussian approximation is made to correlate $c_{av}$ to the experimentally obtained half-width of the resonance curve. In the rotational resonance experiment, the five resonance peaks as predicted by v=- $g_{I}$H- $c_{av}$ $m_{I}$, $m_{I}$=0, $\pm$1 and $\pm$2, were all observed. The magnitude of car was determined by measuring the frequency distance between two adjacent peaks. The sign of $c_{av}$ was determined by the side peak suppression technique. The technique is described, and the sign and magnitude of the spin-rotation constant cav are summarized as following: for C $H_4$ -10.3$\pm$0.4tHz(from the rotational resonance), for SiH +3.71$\pm$0.08kHz(from the nuclear resonance), for Ge $H_4$+3.79$\pm$0.13kHz(from the nuclear resonance), for C $F_4$, -6.81$\pm$0.08kHz(from the rotational resonance), for Si $F_4$, -2.46$\pm$0.06kHz(from the rotational resonance), and finally for Ge $F_4$-1.84$\pm$0.04kHz(from the rotational resonance).onal resonance).esonance).

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Freezing Behaviors of Frozen Foods Determined by $^1H$ NMR and DSC

  • Lee, Su-Yong;Moon, Se-Hun;Shim, Jae-Yong;Kim, Yong-Ro
    • Food Science and Biotechnology
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    • v.17 no.1
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    • pp.102-105
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    • 2008
  • The freezing patterns of commercial frozen foods were characterized by using proton nuclear magnetic resonance ($^1H$ NMR) relaxometry and differential scanning calorimetry (DSC). The liquid-like components like unfrozen water were investigated as a function of temperature (10 to $-40^{\circ}C$) and then compared with the unfrozen water content measured by DSC. The formation of ice crystals and the reduction of water in the foods during freezing were readily observed as a loss of the NMR signal intensity. The proton NMR relaxation measurement showed that the decreasing pattern of the liquid-like components varied depending on the samples even though they exhibited the same onset temperature of ice formation at around $0^{\circ}C$. When compared with the unfrozen water content obtained by the DSC, the NMR and DSC results could be closely correlated at the temperature above $-20^{\circ}C$. However, the distinct divergence in the values between 2 methods was observed with further decreasing temperatures probably due to the solid glass formation which was not detected by DSC.

Backbone NMR assignments of the anti-CRISPR AcrIIA5 from phages infecting Streptococcus thermophilus

  • An, So Young;Kim, Eun-Hee;Bae, Euiyoung;Suh, Jeong-Yong
    • Journal of the Korean Magnetic Resonance Society
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    • v.24 no.3
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    • pp.70-76
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    • 2020
  • The CRISPR-Cas system provides an adaptive immunity for bacteria and archaea against invading phages or foreign plasmids. In the type II CRISPR-Cas system, a single effector protein Cas9 and a guide RNA form an RNA-guided endonuclease complex that can degrade DNA targets of foreign origin. To avoid the Cas9-mediated destruction, phages evolved anti-CRISPR (Acr) proteins that neutralize the host bacterial immunity by inactivating the CRISPR-Cas system. Here we report the backbone 1H, 15N, and 13C resonance assignments of AcrIIA5 that inhibits the endonuclease activity of type II-A Streptococcus thermophilus Cas9 and also Streptococcus pyogenesis Cas9 using triple resonance nuclear magnetic resonance spectroscopy. The backbone chemical shifts of AcrIIA5 predict a disordered region at the N-terminus, followed by an αββββαβββ fold.

$^{31}p$ Nuclear Magnetic Resonance Studies of Acetic Acid Inhibition of Ethanol Production by Strains of Zymomonas mobilis

  • Kim, In-Seop;Barrow, Kevin D.;Rogers, Peter L.
    • Journal of Microbiology and Biotechnology
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    • v.13 no.1
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    • pp.90-98
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    • 2003
  • In vivo $^31p$ Nuclear Magnetic Resonance ($^31p$NMR) and metabolic studies were carried out on an acetic acid tolerant mutant, Zymomonas mobilis $ZM4/Ac^R$, and compared to those of the parent strain, Z. mobilis ZM4, to evaluate possible mechanisms of acetic acid resistance. This investigation was initiated to determine whether or not the mutant strain might be used as a suitable recombinant host far ethanol production from lignocellulose hydrolysates containing various inhibitory compounds. $ZM4/Ac^R$ showed multiple resistance to other lignocellulosic toxic compounds such as syringaldehyde, furfural, hydroxymethyl furfural, vanillin, and vanillic acid. The mutant strain was resistant to higher concentrations of ethanol or lower pH in the presence of sodium acetate, compared to ZM4 which showed more additive inhibition. in vivo $^31p$ NMR studies revealed that intracellular acidification and de-energization were two mechanisms by which acetic acid exerted its inhibitory effect. For $ZM4/Ac^R$, the internal pH and the energy status were less affected by sodium acetate compared to the parent strain. This resistance to pH change and de-energization caused by acetic acid is a possible explanation for the development of resistance by this strain.