• 제목/요약/키워드: Solid state NMR

검색결과 225건 처리시간 0.03초

A Solid-State NMR Study of Water in Poly(vinyl butyral) by Magic Angle Spinning

  • Jeong, Soon-Yong;Han, Oc-Hee
    • Bulletin of the Korean Chemical Society
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    • 제28권4호
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    • pp.662-666
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    • 2007
  • Poly(vinyl butyral) (PVB) with different wt% water was studied gravimetrically as well as with 1H magic angle spinning (MAS) nuclear magnetic resonance (NMR). The composition of PVB samples changes during MAS NMR because of the centrifugal force. As MAS time progresses, initially free water was removed fast but bound water also was gradually depleted. More water was diminished at faster spinning speeds, longer spinning time, higher temperatures, and higher initial water contents. As water in PVB was reduced, the chemical shifts and line widths of different types of water and also those of PVB changed. Our results demonstrate that 1H MAS NMR carried out at 10 kHz in less than about 5 minutes is a convenient and sensitive technique to measure: (a) the content variations of different types of water in polymers, (b) the degree of the interaction of water and polymer, and (c) the molecular dynamics of the polymer. Our study can be extended to different soft polymers with other small molecules than water in them.

Synthesis of New Bicyclic Aziridines Containing Chalcone Analogs and Investigation of Their Photochromic Properties

  • Besharati-Seidani, Tayebeh;Mahmoodi, Nosrat O.
    • Bulletin of the Korean Chemical Society
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    • 제34권3호
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    • pp.875-883
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    • 2013
  • Ten new derivatives of 1,3-diazabicyclo[3.1.0]hex-3-enes linked via ether linkage to chalcones were synthesized and characterized by UV, FT-IR, $^1H$ NMR and $^{13}C$ NMR spectral techniques. The spectra of all synthesized compounds, confirmed structure-photochromic behavior relationships (SPBR) both in solution or in solid state by irradiation under UV light at 254 nm. In other efforts for first time photochromic behavior of ketoaziridines has been investigated.

Recent NMR developments for pharmaceutical research

  • Lee, Kwanghwan
    • 한국자기공명학회논문지
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    • 제20권1호
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    • pp.27-35
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    • 2016
  • NMR spectrometer has been regarded as essential tool for structure elucidation in variable scientific field as like organic synthesis, natural product and macro protein research. Also NMR can be applied for defining dynamic behavior like ligand and receptor binding. One of advantage of research with NMR is that to be great confident to confirm structure and the measured sample could be recovered. Nevertheless NMR also has a weak points than other spectroscopic methods that require a lot of time for interpreting acquired spectrum and running time due to low sensitivity. For last two decade Bruker has developed hardware and software solution for overcome those weak points. In order to overcome low sensitivity Bruker introduced Cryo and Micro diameter probe head technology. And researcher can reduce the time for routine spectrum processing and interpretation works due to lots of introductions in software solutions for quantification, identification and statistics analysis. With four examples, this article describing those new hardware and software solutions in field of recent pharmaceutical research as follows. - New Horizons for NMR in the Biopharmaceutical Industry - The development and application of solid-state NMR spectroscopy (SSNMR) in pharmaceutical analysis - Assisted NMR Data Interpretation in Synthetic Chemistry - Complete Analysis of New Psychoactive Substances Using NMR.

항균성 펩타이드와 혼합된 인지질 분자의 상 변화에 있어서 수화 효과에 대한 고체 핵자기 공명 연구 (A solid-state NMR study on the hydration effect on the lipid phase change in the presence of an antimicrobial peptide)

  • 김철
    • 분석과학
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    • 제26권6호
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    • pp.395-400
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    • 2013
  • 얇은 유리판 위에서 자동적으로 정렬되는 인지질 분자의 정렬도에 대한 수분 및 항균성 펩타이드의 효과를 고체 핵자기 공명 분광법을 이용하여 조사하였다. 순수한 1-palmitoyl-2-oleoyl-sn-glycero-3-phosphotidylcholine (POPC) 인지질 만을 유리판 위에서 정렬시킬 때에는 직접적인 물의 투입 없이 95% 상대 습도에서 수일간 수화시키는 것만으로 충분했다. 하지만, protegrin-1 (PG-1)과 같은 항균성 펩타이드가 혼합되어 있는 인지질의 경우에는 95%의 상대 습도에서 수일간 수화시키는 것과 약간의 물을 시료에 직접 투입하여 수화시키는 것이 크게 달라진다는 것을 확인하였다. 충분한 양의 물이 투입되었을 때, 지질 이중막 위에서 인지질 분자들의 표면 움직임이 매우 활발하였다. 순수한 POPC 분자들이 얇은 유리판 위에서 정렬되는 시간에 비해 항균성 펩타이드가 혼합되어 있는 경우에는 POPC 분자들이 평형상을 이루어질 때까지는 상당한 시간이 필요함을 확인하였다.

에탄올+메탄 하이드레이트에 대한 분광학적 분석연구 (Spectroscopic Analysis of the Ethanol + Methane Hydrate)

  • 이종원;강성필
    • 한국신재생에너지학회:학술대회논문집
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    • 한국신재생에너지학회 2011년도 춘계학술대회 초록집
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    • pp.146.2-146.2
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    • 2011
  • Molecular behaviors and crystal structures of the binary hydrates of $CH_4$ and ethanol were identified by means of 13C solid-state NMR and powder XRD methods at various concentrations of ethanol. In addition, NMR peak areas were used to calculate cage occupancies for both guest species. Obtained results showed that more $CH_4$ molecules are captured into hydrate phase per unit mass of ethanol molecules because $CH_4$ molecule can occupy sII large cages more, and pure $CH_4$ hydrate can form more as well at lower ethanol concentrations. Even though tuning phenomenon was already reported for some aqueous hydrate promoters such as THF, aqueous ethanol solutions are found to play the same tuning role in the binary clathrate hydrates in this study.

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Improved Purification of Thermophilic FoF1-ATP Synthase c-Subunit Rings and Solid-State NMR Characterization of Them in Different Lipid Membranes

  • Bak, Suyeon;Kang, Su-Jin;Suzuki, Toshiharu;Yoshida, Masasuke;Fujiwara, Toshimichi;Akutsu, Hideo
    • 한국자기공명학회논문지
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    • 제17권2호
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    • pp.67-75
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    • 2013
  • ATP synthase produces ATP, a major energy source for metabolic processes in organisms, from ADP and inorganic phosphate in cellular membranes. ATP synthase is known as a rotary motor, in which the c-subunit ring functions as a rotor. In this work, we have tried to develop a more general preparation procedure of thermophilic $F_oc$-ring ($TF_oc$-ring) for NMR measurements. The expression of $TF_oF_1$ is easily affected by various experimental conditions such as temperature, shape and size of a flask, a volume of medium, and shaking rate of an incubator. Accordingly, we have tried to optimize the expression conditions of $TF_oF_1$. $TF_oc$-rings were purified from $TF_oF_1$ according to a reported method. We modified purification procedures to improve purity and yield of $TF_oc$. On top of them, we found a new combination of detergents for the purification at anion-exchange column chromatography. To examine the effect of lipid environments on the structure, the $TF_oc$-rings were reconstituted into two kinds of lipid bilayers, namely, saturated and unsaturated lipid ones. Then, we have compared characteristics of the $TF_oc$-ring structures in these membranes with solid-state NMR.

고분해능 고상 핵자기공명 분광 분석기를 이용한 다성분계 비정질 규산염의 원자 구조 규명: 자연계 용융체의 거시적 성질에 대한 미시적 고찰 (Probing the atomic structure of multi-component silicate glasses using high resolution solid state NMR: microscopic origins of macroscopic properties of natural melts)

  • 박선영;이성근
    • 한국암석학회:학술대회논문집
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    • 한국암석회.한국광물학회 2009년도 공동학술발표회 논문집
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    • pp.29-31
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    • 2009
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