• Title/Summary/Keyword: $^2H$ NMR

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P(3HB) Accumulation in Alcaligenes eutrophus H16(ATCC 17699) under Nutrient-Rich Condition and Its Induced Production from Saccharides and Their Derivatives

  • Song, Jae-Jun;Shin, Yong-Chul
    • Journal of Microbiology and Biotechnology
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    • v.3 no.2
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    • pp.115-122
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    • 1993
  • Poly(3-hydroxybutyrate)(P(3HB)) accumulation under nutrient-rich condition with various amounts of $(NH_4)_2 SO_4$ was systematically investigated. The results of the electron-microscopy and the solvent extraction showed that the P(3HB) accumulation is unavoidable even under nutrient-rich condition. This indicates that in a two-step culture of Alcaligenes eutrophus H16, the researches should be careful in interpreting the data of polyhydroxyalkanoates(PHAs) accumulation in terms of the carbon-source fed in the second step because the two-step culture product contains the P(3HB) produced under nutrient-rich condition. The polyester production capability in a two-step batch culture of A. eutrophus H16(ATCC 17699) was also investigated using various saccharides and their derivatives such as glucose, fructose, gluconic acid, glucaric acid, sorbitol, lactose, galactose, and mannose. The polyesters synthesized were characterized by 500 MHz$^{1}H-NMR$ spectroscopy, intrinsic viscosity$[\eta]$ measurement in chloroform and differential scanning calorimetry(DSC). 500 MHz $^{1}H-NMR$ analysis showed that all polyesters synthesized generally contained 1~2 mol% of 3HV. Another finding is that the glucose utilization can be increased by changing the autoclaving procedure of the substrate to enhance the P(3HB) production yield up to 46 wt% of P(3HB) in dry cells.

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Structural Studies of Copper(II)-Hippuryl-L-histidyl-L-leucine(HHL) Complex by NMR Methods

  • Lee Seong-Ran;Jun Ji-Hyun;Won Ho-Shik
    • Journal of the Korean Magnetic Resonance Society
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    • v.10 no.1
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    • pp.115-125
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    • 2006
  • Hippuryl-L-histidyl-L-leucine(HHL) is widely used as a substrate of angiotensin converting enzyme(ACE) cleaving the neurotransmitter angiotensin(I) to the octapeptide angiotensin(II). The structure of the substrate molecules should provide information regarding the geometric requirements of the ACE active site. For the purpose of determination of in vivo reaction, metallo(Cu, Zn)-HHL complexes were synthesized and the degree of complex formation were identified by MALDITOF, ESI mass spectrometric analysis. Tn addition, the pH-dependent species distribution curves were obtained by potentiometric titration. Nitrogen atoms of imidazole ring and oxygen atom of caboxylate groups in the peptide chain were observed to be participated in the metal complex formation. After purification of complexes further structural characterization were made by utilizing UV-Vis, electrochemical methods and NMR. Complete NMR signal assignments were carried out by using 2D-spectrum techniques COSY, TOCSY, NOESY, HETCOR. A complex that two imidazole and carboxylate groups are asymmetrically participating to coordination mode was predicted to the solution-state structure of $Cu(II)-HHL_2$ based on $^{13}C-NMR$ signal assignment and NOE information.

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Hyperpolarized 129 NMR Study of TiO2 Nanotubes

  • Lee, Sang-Man;Lee, Soon-Chang;Mehrotra, Vandana;Kim, Hae-Jin;Lee, Hee-Cheon
    • Bulletin of the Korean Chemical Society
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    • v.33 no.2
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    • pp.511-514
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    • 2012
  • A continuous flow hyperpolarized (HP) $^{129}Xe$ NMR spectroscopy was employed for the first time to investigate $TiO_2$ nanotubes (Ti-NTs) synthesized from commercial nanoparticles with different reaction times. A single peak attributing to channels for Ti-NTs was observed for variable temperature HP $^{129}Xe$ NMR spectra. It was also noted that there is alteration in value for heat of adsorption, ${\Delta}H$ from $12.6{\pm}1.3$ to $16.4{\pm}0.4kJ/mol$ and variation in chemical shift of the xenon adsorbed in channels, ${\delta}_s$ from $120{\pm}2\sim135{\pm}9ppm$ which were closely correlated to channel length and it was shown that P25-24 Ti-NTs with longest channel is most favorite Ti-NTs for Xe adsorption.

Synthesis of Multisubstrate analog Inhibitor of Thymidylate synthase (Thymidylate Synthesis의 Multisubstrate analog Inhibitor의 합성)

  • Kwak, In-Young;Ryu, Eung-K
    • The Journal of Natural Sciences
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    • v.4
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    • pp.23-28
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    • 1991
  • The pyrimidy1 derivative of 2'-deoxythmidine 5'-monophosphate, 3 has been synthesized for the development of anticanncer agents. The compound 3 derived from prototype inhibitor 2 by modifying the p-aminobenzoy1 glutamic acid portion has been designed to facilitate the membrane penetration. Variable temperature $^1H$ NMR spectrum for the protected nucleotide has indicated the existence of two conformers which are stable on the NMR time scale at ambient temperature.

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Substituted Phenyl 2-Thiophenecarboxylates and Benzoates:Synthesis, NMR Spectra, and Aromaticity Index

  • Lee, Chang Gyu;Yu, Ji Suk;Park, Jong Seok
    • Bulletin of the Korean Chemical Society
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    • v.21 no.1
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    • pp.49-55
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    • 2000
  • A series of m-, and p-substituted phenyl 2-thiophenecarboxylates and benzoates was prepared by the reaction of the corresponding acyl chlorides and phenols. Their $^1H$ and $^{13}C$ NMR chemical shifts were analyzed using single substituent parameter (S SP) and dual substituent parameter (DSP) methods. The relative aromaticity index of thiophene was estimated to be 0.92 from the plot of the chemical shift of the carbonyl carbons of the thienoyl esters against chemical shift of the carbonyl carbons of the benzoyl esters.

Isolation of flavonoids from Rhus verniciflua STOKES

  • Kim, Ho-Kyoung;Lee, A-Yeong;Kim, Jung-Hee;Jeon, Won-Kyung
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.258.2-258.2
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    • 2003
  • Rhus verniciflua STOKES (RVS) belongs to Anacardiaceae and grows Korea, China and Japan. distributed in the northeastern Asia. Rhus verniciflua STOKES has been used for anthelmintic medicine, stomachache, emmenagogue and constipation in oriental medicine. From the EtOAc fraction of 70% MeOH extracts, flavonoids were isolated by column chromatography using ODS, Sephadex LH-20 and silica gel. The structure of these compounds were identified on the $^1$H-NMR, $\^$13/C-NMR and FAB/MS spectroscopic methods.

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Characteristics of Antitumor Antibiotics HS-1 from a Stveptomyces JIoridiae SHS-1372 (Streptomyces floridae SHS-1372가 생산하는 항암항생물질 HS-1의 특성)

  • 하상철;홍순덕
    • Microbiology and Biotechnology Letters
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    • v.22 no.2
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    • pp.169-174
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    • 1994
  • Antitumor antibiotic HS-1 was purified from the culture broth of a streptomyces floridae SHS-1372 which had been isolated from soil, by solvent extraction, silica gel column chromatography and gel filtration. It was confirmed that HS-1 was active against gram positive bacteria and cancer cells(K562, P388, MCF-7, HT-29). Through the analysis of UV spectrum, melting point, IR spectrum, FAB-MS, $_{1}$H-NMR, $_{13}$C-NMR, 2D-NMR spectra, HS-1 could be identified sa the actinomycin X$_{2}$ antibiotics containing actinocine chromophore and peptides consisted of threonine, proline, methylvaline, sarcosine, D-valine and 4-ketoproline.

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Synthesis and Characterization of Stereospecific 1-Propargyl-2-(dimethoxymethyl)-1- cyclohexanols

  • Lin, Juwhan;Kim, Sang-Il;Lee, Seung-Yong;Kim, Yong-Hyun;Lee, Kee-Young;Oh, Chang-Young;Ham, Won-Hun
    • Archives of Pharmacal Research
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    • v.23 no.2
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    • pp.104-111
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    • 2000
  • Stereochemical isomers with hydroxy groups were synthesized by reacting 2-(dimethoxy-methyl)cyclohexanone with propargylmagnesium bromide. The stereo chemical structures were identified by NMR spectral interpretation and the geometry optimization. To assist the NMR interpretation, geometry optimization based on semi-empirical AM1 and PM3 methods was applied. Throughout this study, the structures of the two isomers were all determined and $^{1}H$ and $^{13}C$ NMR spectra were fully assigned. It was proven that the less polar isomer is an axial alcohol and the more polar one is an equatorial alcohol.

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Per-deuteration and NMR experiments for the backbone assignment of 62 kDa protein, Hsp31

  • Kim, Jihong;Choi, Dongwook;Park, Chankyu;Ryu, Kyoung-Seok
    • Journal of the Korean Magnetic Resonance Society
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    • v.19 no.3
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    • pp.112-118
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    • 2015
  • Hsp31 protein is one of the members of DJ-1 superfamily proteins and has a dimeric structure of which molecular weight (MW) is 62 kDa. The mutation of DJ-1 is closely related to early onset of Parkinson's disease. Hsp31 displays $Zn^{+2}$-binding activity and was first reported to be a holding chaperone in E. coli. Its additional glyoxalase III active has recently been characterized. Moreover, an incubation at $60^{\circ}C$ induces Hsp31 protein to form a high MW oligomer (HMW) in vitro, which accomplishes an elevated holding chaperone activity. The NMR technique is elegant method to probe any local or global structural change of a protein in responses to environmental stresses (heat, pH, and metal). Although the presence of the backbone chemical shifts (bbCSs) is a prerequisite for detailed NMR analyses of the structural changes, general HSQC-based triple resonance experiments could not be used for 62 kDa Hsp31 protein. Here, we prepared the per-deuterated Hsp31 and performed the TROSY-based triple resonance experiments for the bbCSs assignment. Here, detailed processes of per-deuteration and the NMR experiments are described for other similar NMR approaches.