• Title/Summary/Keyword: H-NMR

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NMR and Circular Dichroism Studies on Human CD99 Transmembrane Domain

  • Kim, Hai-Young;Shin, Joon;Shin, Young-Kee;Park, Seong-Hoe;Lee, Weon-Tae
    • Journal of the Korean Magnetic Resonance Society
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    • v.7 no.1
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    • pp.37-45
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    • 2003
  • Human CD99 is a ubiquitous 32-kDa transmembrane protein encoded by mic2 gene. Recently it has been reported that expression of a splice variant of CD99 transmembrane protein (Type I and Type II) increases invasive ability of human breast cancer cells. To understand structural basis for cellular functions of CD99 Type II, we have initiated studies on hCD99$\^$TMcytoI/ using circular dichroism (CD) and multi-dimensional NMR spectroscopy. CD spectrum of hCD99$\^$TMytoI/ in the presence of 200mM DPC and CHAPS displayed an existence ${\alpha}$-helical conformation, showing that it could form an ${\alpha}$-helix under membrane environments. In addition, we have found that the cytoplasmic domain of CD99 would form symmetric dimmer in the presence of transmembrane domain. Although it has been rarely figured out the correlation between structure and functional mechanism of hCD99$\^$TMcytoI/, the dimerization or oligomerization would play an important role in its biological function.

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Isolation and Identification of Antimicrobial Compound from Dansam (Saliuia miltiorrhiza Bunge) (단삼으로부터 식품부패미생물에 대한 항균성 물질의 분리 및 동정)

  • 최해연;한영실
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.32 no.1
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    • pp.22-28
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    • 2003
  • Antimicrobial effect of Dansham (Saliuia miltiorrhiza Bunge) was investigated. Methanol extract of dried Dansham was fractionated to hexane, chloroform, ethylacetate, butanol and aqueous fraction. Chloroform fraction showed the highest inhibitory effect on the microorganisms such as B. subtilis, S. aureus, E. coli, L. monocytogenes and V. parahaemolyticus at 250 $\mu\textrm{g}$/disc. Chloroform fraction was further fractionated by silica gel column and thin layer chromatography (TLC). The antimicrobial compound was isolated from their fractions and its chemical structure was identified as a cryptotanshinone by GC-MS and $^1$H-NMR, $^{13}$ C-NMR.

1H-NMR Analysis according to the Storage Period after the Use of Iopamidol and Ioversol Formulations Contrast Agents (Iopamidol과 Ioversol 제제 조영제의 사용 후 보관 기간에 따른 1H-NMR 분석)

  • Han, Beom-Hee
    • Journal of radiological science and technology
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    • v.44 no.3
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    • pp.239-245
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    • 2021
  • Since the side effects of contrast agents occur in many ways, hospitals must clearly identify the contrast agents and know how to manage them. Storage of contrast media It is common practice to store contrast media in a warm room to reduce viscosity and improve patient comfort. However, it is important to recognize that long-term storage at high temperatures can shorten the shelf life of a product. Therefore, in this study, the presence or absence of chemical changes according to the storage period after using the contrast medium was analyzed. As the analysis equipment, a 500 MHz Nuclear Magnetic Resonance Spectrometer of Bruker Avance (Germany) possessed by Korea Basic Science Institute (KOREA BASIC SCIENCE INSTITUTE; KBSI) was used. For the X-ray iodide contrast medium, Pamiray contrast medium of Iopamidol and Optiray contrast medium of Ioversol, samples remaining after 7 days, 20 days, 30 days, and 1 year were collected, By acquiring the spectrum from the 1H-NMR spectrometer of the contrast medium stimulated by It was compared and analyzed with the standard sample. In conclusion, depending on the storage period of the contrast medium, no peaks of physical and chemical changes were observed in both the Pamiray contrast medium of Iopamidol and the Optiray contrast medium of Ioversol after 7 days, 20 days, 30 days, and 1 year after use.

1H-NMR and HPLC analysis on the chiral discrimination of β-blockers using (S)-2-tert-butyl-2-methyl-1,3-benzodioxole-4-carboxylic acid

  • Seo, Sang Hun;Mai, Xuan-Lan;Le, Thi-Anh-Tuyet;Kim, Kyeong Ho
    • Analytical Science and Technology
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    • v.34 no.1
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    • pp.9-16
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    • 2021
  • In the group of commonly prescribed β-blocker drugs, one of the enantiomers is generally relatively more active than the others. This study aims to develop a technique for the chiral analysis of select β-blockers based on proton nuclear magnetic resonance (1H-NMR) spectrometry. (S)-2-Tert-butyl-2-methyl-1,3-benzodioxole-4-carboxylic acid ((S)-TBMB) was synthesized and utilized as a chiral derivatizing agent. Pure β-blocker enantiomers were isolated from racemates by semi-preparative liquid chromatography prior to derivatization. The reaction time and concentration of (S)-TBMB were controlled to improve the derivatization procedure. No racemization was found during the analysis. High-performance liquid chromatography (HPLC) analysis was also performed for comparative purposes. High agreement between the NMR and HPLC methods was achieved in the determination of (R)-metoprolol in a standard solution of the (S) isomer.

Preparation of Trifluoroacetyl Chitosan Derivatives with Antiviral Activity (항바이러스 활성을 갖는 Trifluoroacetyl Chitosan 유도체의 제조)

  • Kim, Chun-Ho;Shin, Cha-Gyun;Shin, Kye-Sook;Son, Tae-il
    • Applied Chemistry for Engineering
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    • v.10 no.4
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    • pp.599-602
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    • 1999
  • Chitosan was depolymerized by using nitrous acid. In order to synthesize new fluorinated chitosan oligomer(FCO) derivative, free amine groups of resulting low molucular weight chitosan oligomers were reacted with trifluoroacetic anhydride. The structure changes in the samples were conformed by using FT-IR, $^{1}H\;NMR$, $^{13}C\;NMR$ and $^{19}F\{^{1}H\}NMR$. Antiviral activity of FCO was studied by measuring DAN amounts of the replication viruses at 36 hr after the cells were infected with the viral solution containing FCO of various concentrations. The viral replications in the cells infected with the viral solution containing FCO were proportionally decreased with the FCO does, compared to those of the control groups, indicating that FCO efficiently inhibits viral infection. In particular, viral replication was decreased to 40% in the 1% FCO-treated cells.

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$^1H$ NMR-Based Urinary Metabolic Profiling of Gender and Diurnal Variation in Healthy Korean Subjects (성별 및 채뇨 시각별 $^1H$ NMR 기반 뇨 대사체 프로파일링 연구)

  • Jeong, Jin-Young;Hwang, Geum-Sook;Park, Jong-Chul;Kim, Dong-Hyun;Ha, Mi-Na
    • Environmental Analysis Health and Toxicology
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    • v.25 no.4
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    • pp.295-306
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    • 2010
  • Objectives : This study was undertaken to examine the metabolomic changes due to gender and diurnal variation at sampling time and to identify an appropriate time point for urine sampling in epidemiologic studies using metabolomic profiles. Methods : Urine samples were collected twice a day (morning and afternoon) from 20 healthy Korean adults after fasting for 8 hours. The metabolomic assay was investigated using $^1H$ NMR spectroscopy coupled with the principal components analysis (PCA) and partial least squares discriminant analysis (PLS-DA). The metabolites responsible for differentiation between groups were identified through the loading plot of PLS-DA and quantified using Chenomx NMR Suite with a 600 MHz library. Results : Metabolites responsible for differentiation in gender and sampling time were creatinine, trimethyl anine oxide (TMAO), hippurate, mannitol, citrate and acetoacetate. Dimethylamine showed difference only as a factor of diurnal time. The level of creatinine was higher in men compared to women, and the levels of citrate, TMAO, hippurate, mannitol, and acetoacetate were higher in women compared to men. The levels of creatinine, TMAO, hippurate, dimethylamine and mannitol were higher in the morning rather than the afternoon while those of citrate and acetoacetate were higher in the afternoon rather than the morning. Conclusions : Since urinary metabolomic profiles varied by gender and diurnal cycle, urine sampling should be performed at the same time point for all participants in epidemiologic studies using metabolomic profiles.

Isolation and Identification of Antimicrobial Compounds from Licorice Extracts (감초 추출물로부터 항균성 물질의 분리 및 동정)

  • Lee, Jin-Man;Lee, Yoon-Won;Hur, Sang-Sun
    • Journal of the Korean Applied Science and Technology
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    • v.33 no.2
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    • pp.255-263
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    • 2016
  • Antimicrobial properties of Licorice(Glycyrrhizae radix L.) against food spoilage microorganism, Bacillus subtilis KCTC 1021 was investigated. Antibacterial activity of the essential oil was as equivalent as Potassium metabisulfite and myconazole. The licorice extracts was fractionated to hexane, chloroform, ethyl acetate, butanol and water fraction. Chloroform fraction showed the highest inhibitory effect on the Bacillus subtilis KCTC 1021. Chloroform fraction was further fractionated by silica gel column chromatography and thin layer chromatography(TLC). The antibacterial compound was isolated from their fractions and its chemical structures was identified as (R)-glabridin by ESI-MS, $^1H$-NMR and $^{13}C$-NMR.

Low-ε Static Probe Development for 15N-1H Solid-state NMR Study of Membrane Proteins for an 800 MHz NB Magnet

  • Park, Tae-Joon;Choi, Sung-Sub;Jung, Ji-Ho;Park, Yu-Geun;Kim, Yongae
    • Bulletin of the Korean Chemical Society
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    • v.34 no.3
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    • pp.823-826
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    • 2013
  • A low-${\varepsilon}$ solid-state NMR(Nuclear Magnetic Resonance) probe was developed for the spectroscopic analysis of two-dimensional $^{15}N-^1H$ heteronuclear dipolar coupling in dilute membrane proteins oriented in hydrated and dielectrically lossy lipid environments. The system employed a 800 MHz narrow-bore magnet. A solenoid coil strip shield was used to reduce deleterious RF sample heating by minimizing the conservative electric fields generated by the double-tuned resonator at high magnetic fields. The probe's design, construction, and performance in solid-state NMR experiments at high magnetic fields are described here. Such high-resolution solid-state NMR spectroscopic analysis of static oriented samples in hydrated phospholipid bilayers or bicelles could aid the structural analysis of dilute biological membrane proteins.

Synthesis and Substituent Effects in Substituted Styryl 4-Methoxy-1-Naphthyl Ketones (다양한 치환기가 붙은 Styryl 4-Methoxy-1-Naphthyl Ketone의 합성과 치환기 효과에 관한 연구)

  • Thirunarayanan, G.;Ananthakrishna Nadar, P.
    • Journal of the Korean Chemical Society
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    • v.50 no.3
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    • pp.183-189
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    • 2006
  • A series of substituted styryl 4-methoxy-1-naphthyl ketones [(2E)-1-(4-methoxy-1-naphthyl)-3-phenyl-2-propen-1-ones] were synthesized using facile method of microwave assisted condensation reaction. The yield of chalcones is more than 90%. They are characterized by their physical constants, micro analysis, infrared (KBr, 4000-400 cm?1) and NMR both 1H and 13C spectral data. From infrared spectra, the s-cis and s-trans stretching vibrations of carbonyl group, from NMR spectra the ethylenic proton and carbon chemical shifts (ppm) are assigned. These spectral data are correlated with various Hammett substituent constants. From the results of statistical analysis the effect of substituents on CO, ? and ? proton and carbons are explained.

[ $^{11}B$ ] Nuclear Magnetic Resonance Study of Spin Structures in Terbium Tetraboride

  • Mean, B.J.;Kang, K.H.;Kim, J.H.;Hyun, I.N.;Lee, Moo-Hee;Cho, B.K.
    • Journal of the Korean Magnetic Resonance Society
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    • v.10 no.2
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    • pp.197-202
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    • 2006
  • [ $^{11}B$ ] nuclear magnetic resonance (NMR) measurements were performed on the single crystals of $TbB_4$ to investigate local electronic structure and 4f spin dynamics. $^{11}B$ NMR spectrum, Knight shift, spin-lattice and spin-spin relaxation rates were measured down to 4K at 8T. $^{11}B$ NMR shift and linewidth are huge and strongly temperature dependent due to the 4f moments. In addition, both are proportional to magnetic susceptibility, indicating that the hyperfine field at the boron site originates from the 4f spins of Tb. Below $T_N$, the single broad resonance peak of $^{11}B$ NMR splits into several peaks reflecting the local magnetic fields due to antiferromagnetic spin arrangements. The longitudinal and the transverse relaxation rates, $1/T_1\;and\;1/T_2$, independent of temperature above $T_N$, decreases tremendously confirming huge suppression of spin fluctuation below $T_N$.

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