• 제목/요약/키워드: Proton nuclear magnetic resonance spectroscopy

검색결과 48건 처리시간 0.023초

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

  • 이승룡;정연복;한건;신재영
    • 약학회지
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    • 제38권3호
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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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인체 뇌 대사물질에서의 In vitro 2D-COSY와 2D-NOESY 스펙트럼 분석 평가 (Evaluations of Spectral Analysis of in vitro 2D-COSY and 2D-NOESY on Human Brain Metabolites)

  • 최보영;우동철;김상영;최치봉;이성임;김은희;홍관수;전영호;정재준;김상수;임향숙
    • Investigative Magnetic Resonance Imaging
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    • 제12권1호
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    • pp.8-19
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    • 2008
  • 목적 : 본 연구에서는 인체 뇌 대사물질에 대하여 2D MR 기술인 correlation spectroscopy (COSY) 와 nuclear Overhauser effect/enhancement spectroscopy (NOESY)를 직접 적용하고, 데이터를 획득하여 인체 뇌대사물질들간의 스칼라 짝지움 (coupling)과 쌍극자 (dipolar) 상호작용- NOE에 대한 분석을 통하여 결합연결관계 및 공간연결관계에 대한 정보를 획득하고자 하였다. 대상 및 방법 : 모든 2-D (dimensional) MR 실험 (즉, COSY와 NOESY)은 z축 능동차폐 펄스경사자장, 삼중공명 동결탐침기가 장착된 Bruker Avance 500 (11.8 T) 장비에서 298 K에 수행되었다. MRS상에서 뇌 대사물질과 유사하도록만든 희석액을 만들었고, 최종 MRS 샘플은 10% $D_2O$를 이용하였다. 2-D 스펙트라는 2048 복합 (complex) 데이터 포인트로서 총 320개 의 free induction decay (FID)를 평균화 (averaging)하였고, $H_2O$에서 얻어진 스펙트라는 8012 Hz 였다. 반복지연 (repetition delay) 시간은 2초, 각각의 FID는 4개의 평균화를 선택하였다. 얻어진 2D-COSY, 2D-NOESY 데이터는 Top Spin 2.0 소프트웨어에서 후 처리기법 (post-processing)에 의해 분석되었다. 분석 대상 대사물질은 N-acetyl aspartate (NAA), creatine (Cr), choline (Cho), glutamine (Gln), glutamate (Glu), myo-inositol (Ins), lactate (Lac)로서 총 7 가지 화학물로서 주요 목표 피크로 정했다. 결과 : 인체 뇌 대사물질에 대한 대칭형태의 2D-COSY와 2D-NOESY 스펙트럼을 획득하였고, COSY 스펙트럼상에서는 오직 1.0-4.5 ppm 사이에서만 교차피크들이 생성된 반면 NOESY 스펙트럼상에서는 1.0-4.5 ppm 외에도 7.9 ppm에서 공명 교차피크를 발견할 수 있었다. COSY 스펙트럼을 통하여 lactate에서 메틸 프로톤과 CH 프로톤의 COSY 크로스피크가 발견되었고, NAA에서 메틸렌 프로톤들간과 메틸렌 프로톤과 NH프로톤의 크로스피크가 발견되었고, Ins에서 CH 프로톤 들간의 크로스피크가 발견되었다. NOESY 스펙트럼을 통하여 NAA 분자내 NH 프로톤과 메틸 (-CH3) 프로톤과의 NOESY 크로스피크가 발견되었고, lactate에서 메틸 프로톤과 CH 프로톤과의 크로스피크가 발견되었고, Cr에서 메틸 프로톤과 메틸렌 프로톤과의 크로스피크가 발견되었고, Glu에서 메틸렌 프로톤 들간과 또한 메틸렌 프로톤과 CH 프로톤과의 크로스피크가 발견되었고, Gln에서 메틸렌 프로톤과 CH 프로톤과의 크로스피크가 발견되었고, Ins에서 CH 프로톤 들간의 크로스피크가 발견되었다. 결론 : 본 연구에서는 in vitro 상태의 인체 뇌 대사물질에 2D-COSY와 2D-NOESY 기술을 직접 적용하고, 결합연결관계 및 공간연결관계에 대한 정보를 성공적으로 획득하여 분석하여 보았다. 본 연구 결과물은 향후 인체 내 in vivo 2D-COSY를 이용한 뇌 대사물질 연구에 매우 유용하리라 사료된다.

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무가습 가교 가지형 공중합체 전해질 막의 제조 (Preparation of Anhydrous Crosslinked Graft Copolymer Electrolyte Membrane)

  • 노동규;고주환;박정태;서진아;김종학
    • 한국신재생에너지학회:학술대회논문집
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    • 한국신재생에너지학회 2009년도 춘계학술대회 논문집
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    • pp.270-273
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    • 2009
  • A comb-like copolymer consisting of a poly(vinylidene fluoride-co-chlorotrifluoro-ethylene) backbone and poly(hydroxy ethyl acrylate) side chains, i.e. P(VDF-co-CTFE)-g-PHEA, was synthesized through atom transfer radical polymerization (ATRP) using CTFE units as a macroinitiator. Successful synthesis and a microphase-separated structure of the copolymer were confirmed by proton nuclear magnetic resonance (1H-NMR), FT-IR spectroscopy, and transmission electron microscopy (TEM). This comb-like polymer was crosslinked with 4,5-imidazole dicarboxylic acid (IDA) via the esterification of the -OH groups of PHEA and the -COOH groups of IDA. Upon doping with phosphoric acid ($H_3PO_4$) to form imidazole-$H_3PO_4$ complexes, the proton conductivity of the membranes continuously increased with increasing $H_3PO_4$ content. A maximum proton conductivity of 0.015 S/cm was achieved at $120^{\circ}C$ under anhydrous conditions. In addition, these P(VDF-co-CTFE)-g-PHEA/IDA/$H_3PO_4$ membranes exhibited good mechanical properties (765 MPa of Young's modulus), and high thermal stability up to $250^{\circ}C$, as determined by a universal testing machine (UTM) and thermal gravimetric analysis (TGA), respectively.

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A Conformational Study of Linkage Positions in Oligosaccharides Investigated by 2-D NMR Spectroscopy and Molecular Modeling

  • Yoo Yoon, Eun-Sun
    • Bulletin of the Korean Chemical Society
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    • 제24권3호
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    • pp.339-344
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    • 2003
  • The conformation of synthetic oligosaccharide can be elucidated by employing molecular modeling and highfield proton NMR (nuclear magnetic resonance) spectroscopy. Information with respect to the composition and configuration of saccharide residues and the sequence and linkage positions of the oligosaccharide can be obtained by employing a variety of one- and two-dimensional NMR techniques and molecular modeling. These techniques are also useful in establishing the solution conformation of the oligosaccharide moiety. This study is focused on the elucidation of linkage positions of synthetic trisaccharides, Gal(β1-4)Glc(β1-3)Glc, Gal(β1-4)Glc(β1-4)Glc and Gal(β1-4)Glc(β1-6)Glc.

Influence of Hot Pressing on the Pore Structure of Nafion Electrolyte Membrane Investigated by 1H NMR

  • Jeonga, Soon-Yong;Han, Oc-Hee
    • Bulletin of the Korean Chemical Society
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    • 제30권7호
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    • pp.1559-1562
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    • 2009
  • The influence of hot pressing on the pore structures of Nafion membranes was investigated by observing the Nafion before and after hot pressing with $^1H$ nuclear magnetic resonance (NMR) spectroscopy. The freezing point depression and chemical shift data of water in the Nafion indicated the presence of two different pore size ranges in Nafion. Hot pressing mainly reduced the sizes and number of the big pores. The reduction of water uptake and proton conductivity after hot pressing was explained by this variation of pore size and number. We demonstrated the potential application of chemical shift data and NMR cryoporometry experiments to measure the relative pore sizes, on a nano scale, and numbers.

Structural and Thermal Analysis and Membrane Characteristics of Phosphoric Acid-doped Polybenzimidazole/Strontium Titanate Composite Membranes for HT-PEMFC Applications

  • Selvakumar, Kanakaraj;Kim, Ae Rhan;Prabhu, Manimuthu Ramesh;Yoo, Dong Jin
    • Composites Research
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    • 제34권6호
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    • pp.373-379
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    • 2021
  • A series of novel PBI/SrTiO3 nanocomposite membranes composed of polybenzimidazole (PBI) and strontium titanate (SrTiO3) with a perovskite structure were fabricated with various concentrations of SrTiO3 through a solution casting method. Various characterization techniques such as proton nuclear magnetic resonance, thermogravimetric analysis, atomic force microscopy (AFM) and AC impedance spectroscopy were used to investigate the chemical structure, thermal, phosphate absorption and morphological properties, and proton conductivity of the fabricated nanocomposite membranes. The optimized PBI/SrTiO3-8 polymer nanocomposite membrane containing 8wt% of SrTiO3 showed a higher proton conductivity of 7.95 × 10-2 S/cm at 160℃ compared to other nanocomposite membranes. The PBI/SrTiO3-8 composite membrane also showed higher thermal stability compared to pristine PBI. In addition, the roughness change of the polymer composite membrane was also investigated by AFM. Based on these results, nanocomposite membranes based on perovskite structures are expected to be considered as potential candidates for high-temperature PEM fuel cell applications.

Improving dispersion of multi-walled carbon nanotubes and graphene using a common non-covalent modifier

  • Kwon, Youbin;Shim, Wonbo;Jeon, Seung-Yeol;Youk, Ji-Ho;Yu, Woong-Ryeol
    • Carbon letters
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    • 제20권
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    • pp.53-61
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    • 2016
  • The reportedly synergistic effects of carbon nanotubes (CNTs) and graphene hybrids have prompted strong demand for an efficient modifier to enhance their dispersion. Here, we investigated the ability of poly(acrylonitrile) (PAN) to overcome the van der Waals interaction of multi-walled CNTs (MWCNTs) and graphene by employing a simple wrapping process involving ultrasonication and subsequent centrifugation of PAN/MWCNT/graphene solutions. The physical wrapping of MWCNTs and graphene with PAN was investigated for various PAN concentrations, in an attempt to simplify and improve the polymer-wrapping process. Transmission electron microscopy analysis confirmed the wrapping of the MWCNTs and graphene with PAN layers. The interaction between the graphitic structure and the PAN molecules was examined using proton nuclear magnetic resonance, ultraviolet-visible spectroscopy, Fourier transform infrared spectroscopy, thermogravimetric analysis, and Raman spectroscopy. The obtained results revealed that the cyano groups of the PAN molecules facilitated adhesion of the PAN molecules to the MWCNTs and graphene for polymer wrapping. The resulting enhanced dispersion of MWCNTs and graphene was verified from zeta potential and shelf-life measurements.

Synthesis and Properties of Combined Main-Chain/Side-Chain Liquid Crystalline Polymers with Cholesteryl and Azobenzene Groups

  • Gu, Su-Jin;Lee, Eung-Jae;Bang, Moon-Soo
    • Elastomers and Composites
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    • 제54권1호
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    • pp.14-21
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    • 2019
  • Main-chain/side-chain liquid crystalline polymers (MCSCLCPs) combined with an azobenzene group and a cholesteryl group were synthesized to impart light and temperature sensitivity to the polymer. The polymers were designed with the azobenzene unit as the mesogenic group of the main-chain and various compositions of the azobenzene and cholesteryl units as the mesogenic group of the side-chain. The chemical structures and physical properties of the synthesized polymers were investigated by Fourier transform infrared spectroscopy, proton nuclear magnetic resonance spectroscopy, differential scanning calorimetry, thermogravimetric analysis, polarized optical microscopy, and ultraviolet-visible (UV-Vis) spectroscopy. All the MCSCLCPs were amorphous and exhibited enantiotropic liquid crystal phases; these polymers achieved the nematic phase with increasing content of the azobenzene group and exhibited the cholesteric phase with weak liquid crystallinity as the content of the cholesteryl group was increased. Furthermore, the polymers containing the azobenzene group showed photoisomerization when exposed to UV-Vis light, and the CP-A3C7 and CP-A5C5 polymers exhibited thermochromism in the temperature range of the liquid crystal phase.

정상 위 조직과 위암 조직의 시험관 내 수소자기공명분광 (Ex Vivo ${1}^H$ MR Spectroscopy: Normal gastric and cancer tissue)

  • 조지연;신운재;최기승;김수현;은충기;양영일;이정희;문치웅
    • Journal of Gastric Cancer
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    • 제3권3호
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    • pp.151-157
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    • 2003
  • Purpose: In this study, we attempted to ascertain the proton magnetic resonance spectroscopy (${1}^H$ MRS) peak characteristics of human gastric tissue layers and finally to use the metabolic peaks of MRS to distinguish between normal and abnormal gastric specimens. Materials and Methods: Ex-vivo ${1}^H$ MRS examinations of thirty-five gastric specimens were performed to distinguish abnormal gastric tissues invaded by carcinoma cells from normal stomach-wall tissues. High-resolution 400-MHz (9.4-T) ${1}^H$ nuclear magnetic resonance (NMR) spectra of two gastric layers, a proper muscle layer, and a composite mucosasubmucosa layer were compared with those of clinical 64- MHz (1.5-T) MR spectra. Three-dimensional spoiled gradient recalled (SPGR) images were used to determine the size and the position of a voxel for MRS data collection. Results: For normal gastric tissue layers, the metabolite peaks of 400-MHz ${1}^H$ MRS were primarily found to be as follows: lipids at 0.9 ppm and 1.3 ppm; alanine at 1.58 ppm; N-acetyl neuraminic acid (sialic acid) at 2.03 ppm; and glutathione at 2.25 ppm in common. The broad and featureless featureless spectral peaks of the 64-MHz MRS were bunched near 0.9, 1.3, and 2.0, and 2.2 ppm in human specimens without respect to layers. In a specimen (Borrmmann type III) with a tubular adenocarcinoma, the resonance peaks were measured at 1.26, 1.36 and 3.22 ppm. All the peak intensities of the spectrum of the normal gastric tissue were reduced, but for gastric tumor tissue layers, the lactate peak split into 1.26 and 1.39 ppm, and the peak intensity of choline at 3.21 ppm was increased. Conclusion: We found that decreasing lipids, an increasing lactate peak that split into two peaks, 1.26 ppm and 1.36 ppm, and an increasing choline peak at 3.22 ppm were markers of tumor invasion into the gastric tissue layers. This study implies that MR spectroscopy can be a useful diagnostic tool for gastric cancer.

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