• Title/Summary/Keyword: Proton Nuclear Magnetic Resonance

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Synthesis and Characterization of Fluorinated Polybenzimidazole Proton Exchange Membranes for Fuel Cell (연료전지용 불소화 폴리벤즈이미다졸 양성자 교환 멤브레인 합성 및 특성평가)

  • KIM, AE RHAN
    • Transactions of the Korean hydrogen and new energy society
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    • v.28 no.1
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    • pp.24-29
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    • 2017
  • A fluorinated polybenzimidazole (FPBI) was synthesized from 3,3-diaminobenzidine (DAB) of tetraamine, 2,2-bis(4-carboxyphenyl)hexafluoropropane of aromatic biscarboxylic acid, and 4,4-sulfonyldibenzoic acid of aromatic biscarboxylic acid in polyphosphoric acid (PPA). A FPBI was easily cast and made into clear films. The structure of condensation polymers and corresponding membranes were analyzed using GPC (gel permeation chromatography), $^1H$-NMR ($^1H$ nuclear magnetic resonance) and FT-IR (fourier transform infrared). TGA (thermogravimetric analysis) analysis showed that the prepared membranes were thermally stable, so that elevated temperature fuel cell operation would be possible. The proton conductivity of the FPBI membranes increased with increasing temperatures in the polymer. A FPBI membrane has a maximum ion conductivity of 45 mS/cm at $90^{\circ}C$ and 100% relative humidity.

Assignment of ¹H and $^{13}C$ Nuclear Magnetic Resonances of Ganglioside $G_{A1}$

  • 이경익;전길자;류경임;방은정;최병석;김양미
    • Bulletin of the Korean Chemical Society
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    • v.16 no.9
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    • pp.864-869
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    • 1995
  • Investigation of the structures of the gangliosides has proven to be very important in the understanding of their biological roles such as regulation of differentiation and growth of cells. We used nuclear magnetic resonance spectros-copy in order to investigate the structure of GA1. In order to do this, the assignment of spectra is a prerequisite. Since GA1 does not have polar sialic acid, the spectral overlap is severe. In order to solve this problem, we use 2D NMR spectroscopy and heteronuclear 1H/13C correlated spectroscopy in this study. Here, we report the complete assignment of the proton and the carbon spectra of the GA1 in DMSO-d6-D20 (98:2, v/v). These assignments will be useful for interpreting 1H and 13C NMR data from uncharacterized oligosaccharides and for determining the linkage position, the number of sugar rings, and the sequence of new ganglioside. Amide proton in ring Ⅲ shows many interring nOes and has intramolecular hydrogen bonding. This appears to be an important factor in tertiary folding of GA1. Based on this assignment, determination of three dimensional structure of GA1 will be carried out. Studies on the conformational properties of GA1 may lead to a better understanding of the molecular basis of its functions.

Dichlororhodium(Ⅲ) Complexes of N,N$^\prime$-Dimethylethylenediamine-N,N$^\prime$-diacetic Acid

  • Kim, Chang-Hwan;Jun, Moo-Jin;Jun, Jin-Seung
    • Bulletin of the Korean Chemical Society
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    • v.7 no.2
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    • pp.145-147
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    • 1986
  • Dichlororhodium(Ⅲ) complexes of a flexible quadridentate ligand, N,N'-dimethylethylenediamine-N,N'-diacetic acid (dmedda), have been prepared. Both cis-${\alpha}$ and cis-${\beta}$ isomers have been yielded in the $K[Rh(dmedda)Cl_2]$ complexes, which were characterized with elemental analyses, electronic absorption and proton nuclear magnetic resonance spectroscopic data.

Proton and Deuteron Spin-Lattice Relaxation in Gaseous HD (HD 기체에서의 수소 및 중수소 원자핵 스핀-격자 완화시간에 관한 핵자기공명 연구)

  • ;R. E. Norberg
    • Journal of the Korean Magnetics Society
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    • v.4 no.1
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    • pp.52-55
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    • 1994
  • The proton and deuteron spin-lattice relaxation times, $T_{1}(H)$ and $T_{1}(D)$, have been measured in HD between 30 K and 313 K in the pressure of 0.67 - 1.92 atm. The nuclear magnetic resonance frequencies are respectively 358.012 MHz for a proton and 58.958 MHz for a deuteron. From the measurements of $T_{1}(H)$ and $T_{1}(D)$ the ratio of the correlation times ${\tau}_{1}\;and\;{\tau}_{2}$ that are associated with the molecular angular momentum operators was obtained. The nuclear spin-lattice relaxation time at J = 1 state has been observed to have a temperature dependence being proportional to $T^{0.25}$.

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Comparison of Physicochemical Properties between Ursodeoxycholic Acid and Chenodeoxycholic Acid Inclusion Complexes with ${\beta}-Cyclodextrin$ (우르소데옥시콜린산 및 케노데옥시콜린산의 베타시클로덱스트린 포접복합체의 물리화학적 특성비교)

  • Lee, Seung-Yong;Chung, Youn-Bok;Han, Kun;Shin, Jae-Young
    • YAKHAK HOEJI
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    • v.38 no.3
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    • pp.300-310
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    • 1994
  • Physicochemical properties for the inclusion complex of chenodeoxycholic acid(CDCA) and it's $7{\beta}-hydroxy$ epimer ursodeoxycholic acid(UDCA) with ${\beta}-cyclodextrin({\beta}-CyD)$ were studied. The formation of the complex in the solid state were confimed by polarized microscopy and differential scanning calorimetry(DSC). Proton nuclear magnetic resonance$(^1H-NMR)$spectroscopy showed that CDCA and UDCA form an inclusion complex with ${\beta}-CyD$ in aqueous solution. The 1 : 1 stoichiometry of the complex was dextermined by the continuous variation method. From DSC and $^1H-NMR$ studies, there were not any differences between CDCA and UDCA. Complex of CDCA and UDCA showed increase in solubility and dissolution compared with CDCA and UDCA alone, respectively. Solubility pattern of UDCA complex was pH independent but, CDCA complex was like that of CDCA. Dissolution rate increased markedly in case of UDCA complex compared with CDCA complex, especially in acidic pH value.

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1D Proton NMR Spectroscopic Determination of Ethanol and Ethyl Glucuronide in Human Urine

  • Kim, Siwon;Lee, Minji;Yoon, Dahye;Lee, Dong-Kye;Choi, Hye-Jin;Kim, Suhkmann
    • Bulletin of the Korean Chemical Society
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    • v.34 no.8
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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.

Metabolomics comparison of serum and urine in dairy cattle using proton nuclear magnetic resonance spectroscopy

  • Eom, Jun Sik;Kim, Eun Tae;Kim, Hyun Sang;Choi, You Young;Lee, Shin Ja;Lee, Sang Suk;Kim, Seon Ho;Lee, Sung Sill
    • Animal Bioscience
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    • v.34 no.12
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    • pp.1930-1939
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    • 2021
  • Objective: The aim of the study was to conduct metabolic profiling of dairy cattle serum and urine using proton nuclear magnetic resonance (1H-NMR) spectroscopy and to compare the results obtained with those of other dairy cattle herds worldwide so as to provide a basic dataset to facilitate research on metabolites in serum and urine. Methods: Six dairy cattle were used in this study; all animals were fed the same diet, which was composed of total mixed ration; the fed amounts were based on voluntary intake. Blood from the jugular neck vein of each steer was collected at the same time using a separate serum tube. Urine samples were collected by hand sweeping the perineum. The metabolites were determined by 1H-NMR spectroscopy, and the obtained data were statistically analyzed by performing principal component analysis, partial least squares-discriminant analysis, variable importance in projection scores, and metabolic pathway data using Metaboanalyst 4.0. Results: The total number of metabolites in the serum and urine was measured to be 115 and 193, respectively, of which 47 and 81, respectively were quantified. Lactate (classified as an organic acid) and urea (classified as an aliphatic acylic compound) exhibited the highest concentrations in serum and urine, respectively. Some metabolites that have been associated with diseases such as ketosis, bovine respiratory disease, and metritis, and metabolites associated with heat stress were also found in the serum and urine samples. Conclusion: The metabolites measured in the serum and urine could potentially be used to detect diseases and heat stress in dairy cattle. The results could also be useful for metabolomic research on the serum and urine of ruminants in Korea.

Metabolomics comparison of rumen fluid and milk in dairy cattle using proton nuclear magnetic resonance spectroscopy

  • Eom, Jun Sik;Kim, Eun Tae;Kim, Hyun Sang;Choi, You Young;Lee, Shin Ja;Lee, Sang Suk;Kim, Seon Ho;Lee, Sung Sill
    • Animal Bioscience
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    • v.34 no.2
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    • pp.213-222
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    • 2021
  • Objective: The metabolites that constitute the rumen fluid and milk in dairy cattle were analyzed using proton nuclear magnetic resonance (1H-NMR) spectroscopy and compared with the results obtain for other dairy cattle herds worldwide. The aim was to provide basic dataset for facilitating research on metabolites in rumen fluid and milk. Methods: Six dairy cattle were used in this study. Rumen fluid was collected using a stomach tube, and milk was collected using a pipeline milking system. The metabolites were determined by 1H-NMR spectroscopy, and the obtained data were statistically analyzed by principal component analysis, partial least squares discriminant analysis, variable importance in projection scores, and metabolic pathway data using Metaboanalyst 4.0. Results: The total numbers of metabolites in rumen fluid and milk were measured to be 186 and 184, and quantified as 72 and 109, respectively. Organic acid and carbohydrate metabolites exhibited the highest concentrations in rumen fluid and milk, respectively. Some metabolites that have been associated with metabolic diseases (acidosis and ketosis) in cows were identified in rumen fluid, and metabolites associated with ketosis, somatic cell production, and coagulation properties were identified in milk. Conclusion: The metabolites measured in rumen fluid and milk could potentially be used to detect metabolic diseases and evaluate milk quality. The results could also be useful for metabolomic research on the biofluids of ruminants in Korea, while facilitating their metabolic research.

Blood and milk metabolites of Holstein dairy cattle for the development of objective indicators of a subacute ruminal acidosis

  • Hyun Sang Kim;Jun Sik Eom;Shin Ja Lee;Youyoung Choi;Seong Uk Jo;Sang Suk Lee;Eun Tae Kim;Sung Sill Lee
    • Animal Bioscience
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    • v.36 no.8
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    • pp.1199-1208
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    • 2023
  • Objective: The purpose of this study was to perform a comparative analysis of metabolite levels in serum and milk obtained from cows fed on different concentrate to forage feed ratios. Methods: Eight lactating Holstein cows were divided into two groups: a high forage ratio diet (HF; 80% Italian ryegrass and 20% concentrate of daily intake of dry matter) group and a high concentrate diet (HC; 20% Italian ryegrass and 80% concentrate) group. Blood was collected from the jugular vein, and milk was sampled using a milking machine. Metabolite levels in serum and milk were estimated using proton nuclear magnetic resonance and subjected to qualitative and quantitative analyses performed using Chenomx 8.4. For statistical analysis, Student's t-test and multivariate analysis were performed using Metaboanalyst 4.0. Results: In the principal component analysis, a clear distinction between the two groups regarding milk metabolites while serum metabolites were shown in similar. In serum, 95 metabolites were identified, and 13 metabolites (include leucine, lactulose, glucose, betaine, etc.) showed significant differences between the two groups. In milk, 122 metabolites were identified, and 20 metabolites (include urea, carnitine, acetate, butyrate, arabinitol, etc.) showed significant differences. Conclusion: Our results show that different concentrate to forage feed ratios impact the metabolite levels in the serum and milk of lactating Holstein cows. A higher number of metabolites in milk, including those associated with milk fat synthesis and the presence of Escherichia coli in the rumen, differed between the two groups compared to that in the serum. The results of this study provide a useful insight into the metabolites associated with different concentrate to forge feed ratios in cows and may aid in the search for potential biomarkers for subacute ruminal acidosis.