• 한국자기공명학회논문지
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• 제11권2호
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• pp.64-72
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• 2007

[ $^1H$ ] nuclear magnetic resonance (NMR) experiments have been performed at 30 - 300 K and 7 T to investigate dynamics of hydrogen bond network in the single crystal $(NH_4)_3H(SO_4)_2$. The two proton sites, ammonium proton and hydrogen-bond proton, are identified from the $^1H$ NMR MAS spectrum at 340 K. As temperature decreases, the $^1H$ NMR spectrum shifts to the higher frequency side with a larger linewidth. The spectrum at 65 K shows a distinctive change in line shape toward the ferroelectric transition at 63 K. The measured values of $T_1$ for ammonium and hydrogen-bond protons are similar in the whole range of temperature. $T_1$ of $^1H$ NMR shows a gradual decrease down to 120 K and starts to steeply increase below 100 K. Then $T_1$ shows abrupt decrease below 70 K with a sharp minimum at 63 K, where the ferroelectric transition occurs. This temperature dependence of spectrum and $T_1$ clearly prove that the large change in the dynamics of hydrogen bond network is associated with the ferroelectric phase transition at 63 K.

• 한국자기공명학회논문지
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• 제19권2호
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• pp.88-94
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• 2015

Bub1 is one of the spindle checkpoint proteins and plays a role in recruitment of the related proteins to kinetochore. Here, we studied the structural characteristic of the evolutionarily conserved 160 amino acid region in the N-terminus (hBub1 CD1), using Circular Dichroism (CD) and NMR. Our CD results showed that hBub1 CD1 is a highly helical protein and its structure was affected by pH: as pH was elevated to basic pH, the helical propensity increased. This could be related to the surface charge of the hBub1 CD1. However, the structural change did not largely depend on the salt concentration, though the thermal stability a little increased. The previous NMR analysis revealed that the hBub1 CD1 adopts eight helices, which is consistent with the CD result. Our result would be helpful for evaluating the molecular mechanism of the hBub1 CD1 and protein-protein interactions.

• Journal of Microbiology and Biotechnology
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• 제15권6호
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• pp.1330-1336
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• 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.

• Bulletin of the Korean Chemical Society
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• 제29권1호
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• pp.81-84
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• 2008

In the present study, we report 1H and 13C NMR data of 19 methoxyflavonol derivatives with different substitution patterns on A- and B-ring. In addition, the influence of the methoxy substituents in A- and B-ring on the 1H and 13C NMR chemical shifts is discussed: the 1H and 13C chemical shifts of and the number of methoxyl groups provided information allowing elimination of many structural isomers from consideration and in certain instances greatly simplified structural elucidation.

• 한국산학기술학회논문지
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• 제19권12호
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• pp.814-824
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• 2018

거세한우 3두를 $3{\times}3$ Latin square design 시험방법에 적용하여 사료 적응 기간 10일 후 사료 급여 방식에 따른 반추위액 내 휘발성지방산과 단당류 비교 분석 및 대사산물 분석에 대한 연구를 수행하였다. 연구 결과 HPLC와 HPAEC에서 측정되지 않은 휘발성지방산과 단당류들은 $^1H-NMR$에서는 측정이 가능 한 것을 알 수 있었다. $^1H-NMR$에서 측정된 대사산물 중, carbohydrate 계열 대사산물 pyruvate는 사료 급여 전 반추위액에서만 측정 되었으며, succinate는 사료 급여 전 후에서 모두 측정 되었다. Amino acid 계열 대사산물은 총 9가지가 측정 되었다. Lipid 계열 대사산물 ethylene glycol는 사료 급여 전 Con구에서 유의적(P<0.05)으로 높게 측정 되었다. Aiphatic acylic compounds 계열 대사산물 trimethylamine N-oxide는 유의적인 차이는 보이지 않았다. 이번 연구를 통해 $^1H-NMR$를 이용하여 반추위액 내 많은 대사산물 측정이 가능한 것을 알 수 있었으며 사료 급여 전 후 급여 방식에 따라 대사산물의 변화가 나타나는 것을 확인 할 수 있었다.

• Archives of Pharmacal Research
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• 제19권4호
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• pp.302-306
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• 1996

The $^1H- and^{13}C-NMR$ spectra of alaternin, aurantio-obtusin, chryso-obtusin, obtusin and 2-glucosyl obtusifolin isolated from the seeds of Cassia tora have been assigned based on HMBC, long-range HETCOR, fully $^1H-coupled {13}^C-NMR$, deuterium isotope experiment, and by comparison with the model compounds.

• 분석과학
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• 제13권1호
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• pp.49-54
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• 2000

5단계 반응을 통하여 실리카겔의 8-hydroxyquinoline 유도체를 제조하였으며, 각 단계에서 얻은 생성물들을 IR과 NMR을 이용하여 분석하였다. 실리카겔 자체에 관한 IR 스펙트럼으로부터, 자유 hydroxyl기와 수소 결합된 hydroxyl기가 존재하는 것을 확인할 수 있었다. 첫 단계 반응에서는 N-H와 C-H의 IR 밴드와 APTS기에 있는 메틸렌 탄소의 NMR peak을 확인하였다. 둘째 단계에서는 카보닐, nitro, 방향족 탄소의 IR 밴드와 지방족, 방향족, 카보닐 탄소의 NMR peak을 관찰하였으며, 셋째 단계에서 $NO_2$가 $NH_2$로 환원되는 것을 IR과 NMR로 확인할 수 있었다. 마지막 단계에서는 4번째 단계에서 생성된 $N{\equiv}N$ IR peak이 사라지는 것으로부터 8-quinolinol이 고정화되는 것을 확인할 수 있었다.

• Bulletin of the Korean Chemical Society
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• 제13권2호
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• pp.135-139
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• 1992

The mono(aryl)cyanoplatinum(II) complex $[Pt(CN)(C_6H_3{CH_2NMe_2}_2-26)]$, reacts with the dihalogens to yield the mono(aryl)cyanoplatinum complexes $[PtX_2(CN)(C_6H_3{CH_2NMe_2}_2-26)]$, (X = Cl, Br, I). The structural configuration of the two halogen atoms for a square planar platinum complex was studied by 1H-NMR spectroscopy and led to a mixture of trans and cis orientation. The trans orientation was found to be more stable in energy (1.33 kcal/mol) than the cis orientation by means of Extended H ckel calculations. On the base of a combination of the analysis of $^1H-NMR$, $^{13}C-NMR spectra and computational calculations it is assumed that the intermediate consists of an initial attack in the linear transition state, leading to the $S_{N}2$ type mechanism.

• Bulletin of the Korean Chemical Society
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• 제34권8호
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• pp.2413-2418
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• 2013

Forensic and legal medicine require reliable data to indicate excessive alcohol consumption. Ethanol is oxidatively metabolized to acetate by alcohol dehydrogenase and non-oxidatively metabolized to ethyl glucuronide (EtG), ethyl sulfate (EtS), phosphatidylethanol, or fatty acid ethyl esters (FAEE). Oxidative metabolism is too rapid to provide biomarkers for the detection of ethanol ingestion. However, the non-oxidative metabolite EtG is a useful biomarker because it is stable, non-volatile, water soluble, highly sensitive, and is detected in body fluid, hair, and tissues. EtG analysis methods such as mass spectroscopy, chromatography, or enzyme-linked immunosorbent assay techniques are currently in use. We suggest that nuclear magnetic resonance (NMR) spectroscopy could be used to monitor ethanol intake. As with current conventional methods, NMR spectroscopy doesn't require complicated pretreatments or sample separation. This method has the advantages of short acquisition time, simple sample preparation, reproducibility, and accuracy. In addition, all proton-containing compounds can be detected. In this study, we performed $^1H$ NMR analyses of urine to monitor the ethanol and EtG. Urinary samples were collected over time from 5 male volunteers. We confirmed that ethanol and EtG signals could be detected with NMR spectroscopy. Ethanol signals increased immediately upon alcohol intake, but decreased sharply over time. In contrast, EtG signal increased and reached a maximum about 9 h later, after which the EtG signal decreased gradually and remained detectable after 20-25 h. Based on these results, we suggest that $^1H$ NMR spectroscopy may be used to identify ethanol non-oxidative metabolites without the need for sample pretreatment.

• Applied Biological Chemistry
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• 제47권2호
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• pp.270-273
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• 2004

꾸지뽕나무(Cudrania tricuspidata Bureau)의 클로로포름 추출물로부터 2종의 prenylated flavonoid 항균 물질을 분리하였다. 분리할 화합물에 대하여 항균활성을 실험 한 결과 화합물 1과 2는 $10\;{\mu}g/disk$의 농도에서 Gram 양성균인 Staphylococcus aureus, Bacillus subtilis 그리고 Bacillus cereus에 대하여 활성을 보였다. 이들의 구조를 $^lH\;NMR,\;^{13}C\;NMR$ 및 2D NMR을 포함한 분광학적인 방법을 통하여 분석한 결과, 화합물 1과 2는 euchrestaflavanone B와 euchrestaflavanone C로 각각 동정 되었다.