• 제목/요약/키워드: 31P NMR

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파두와 황련의 수용성 혼합물$(CP_2)$부터 분리된 항암성분의 구조확인 및 세포독성에 대한 연구 (Identification of Active Component Isolated from Croton tiglium and Coptis japonica Aqueous Mixture$(CP_2)$ and Studies of Its Cytotoxic Effect)

  • 김정한;이상준;한영복;김종배
    • 약학회지
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    • 제38권1호
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    • pp.31-37
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    • 1994
  • Active fraction, $P_2$, was Isolated from natural anti-cancer drug, $CP_2$, by HPLC. We confirmed that $P_2$ includes most of the Isoguanosine and minor components, Berberine and other protoberberine alkaloids, by $^1H-NMR$ and $^{13}C-NMR$ and measured tile cytotoxicity of $P_2$ against various tumor cell-lines.' $P_2$ was very effective to all tumor cell-lines, especially to human colon cancer SNU-C2A$(ED_{50};\;24{\mu}g)$ and liver cancer HEP-3B$(ED_{50};\;27{\mu}g)$.

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몇가지 $d^8$ 전이금속-디포스핀 착물 ($MCl_2PP$)의 합성과 촉매적 응용 (M = $Ni^{2+}$, $Pd^{2+}$, $Pt^{2+}$, $Au^{3+}$ ; PP = diphosphines) (Synthesis Catalytic Application of Several$d^8Transition Metal Diphosphine Complexes, (MCl_2PP) (M = Ni^{2+}, Pd^{2+}, Pt^{2+}, Au^{3+} ; PP = diphosphines)$)

  • 박유철;김경채;조영제
    • 대한화학회지
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    • 제36권5호
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    • pp.685-691
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    • 1992
  • 디포스핀을 포함한 몇가지 $d^8$ 전이금속착물$(MCl_2PP)$은 출발물질 $K_nMCl_m$을 사용하여 합성하였다. 중심금속(M)은 Ni(II), Pd(II), Pt(II), Au(III)이며, 디포스핀(PP)은 bis(diphenylphosphino)methane(dppm), bis(diphenylphosphino)ethane(dppe), bis(diphenylphosphino)propane (dppp) 및 bis(diphenylphosphino)ethylene(dppety)이었다. 착물의 조성이나 특성은 원소분석과 $^1H-NMR$, $^{31}P-NMR$ 및 UV-Visible 스펙트럼을 이용하여 확인하였다. 이들 착물의 촉매적 활성은 3(2H)-furanone 및 cyclic carbonate 생성반응에 대하여 각각 조사하였다. 2-methyl-3-butyn-2-ol로부터 생성물 3(2H)-furanone을 얻은 반응 (1)에서 Ni(II)-, Pd(II)-diphosphine 착물은 좋은 촉매적 효과를 나타내었다. 그러나 이들 diphosphine 착물들은 cyclic carbonate 생성반응 (2)에 대해 촉매제로서의 활성을 거의 나타내지 않았다.

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Dosage Effects of Salt and pH Stresses on Saccharomyces cerevisiae as Monitored via Metabolites by Using Two Dimensional NMR Spectroscopy

  • Chae, Young Kee;Kim, Seol Hyun;Ellinger, James E.;Markley, John L.
    • Bulletin of the Korean Chemical Society
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    • 제34권12호
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    • pp.3602-3608
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    • 2013
  • Saccharomyces cerevisiae, which is a common species of yeast, is by far the most extensively studied model of a eukaryote because although it is one of the simplest eukaryotes, its basic cellular processes resemble those of higher organisms. In addition, yeast is a commercially valuable organism for ethanol production. Since the yeast data can be extrapolated to the important aspects of higher organisms, many researchers have studied yeast metabolism under various conditions. In this report, we analyzed and compared metabolites of Saccharomyces cerevisiae under salt and pH stresses of various strengths by using two-dimensional NMR spectroscopy. A total of 31 metabolites were identified for most of the samples. The levels of many identified metabolites showed gradual or drastic increases or decreases depending on the severity of the stresses involved. The statistical analysis produced a holistic outline: pH stresses were clustered together, but salt stresses were spread out depending on the severity. This work could provide a link between the metabolite profiles and mRNA or protein profiles under representative and well studied stress conditions.

Synthesis of Dendrimer Based Polymeric and Macrocyclic Complexes with a Platinum-Acetylide ${\pi}-Conjugated$ Organometallic Core

  • Jang, Woo-Dong
    • Macromolecular Research
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    • 제13권4호
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    • pp.334-338
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    • 2005
  • A three-layered poly(benzyl ether) dendrimer having a bis-ethynylbenzene core was synthesized and characterized with $^{1}H$ NMR and MALDI-TOF-MS spectroscopy. The dendrimer was reacted with platinum complexes to obtain platinum-acetylide based organometallic polymers. When the dendrimer was reacted with trans-[$PtCl_{2}(PEt_{3})_{2}$], a high molecular weight polymeric compound was formed, whereas, with cis-[$PtCl_{2}dppp$], a uniform molecular weight compound was formed, which was found to be a dimeric metallacycle by $^{1}H\;NMR,\;^{31}P\;NMR$ and ESI-TOF-MS spectroscopy. Both these complexes exhibited relatively a strong emission around 440 nm, indicating that they could be potential candidates for blue emitting polymer LEDs.

Overexpression and Spectroscopic Characterization of a Recombinant Human Tumor Suppressor p16INK4

  • Lee, Weon-Tae;Jang, Ji-Uk;Kim, Dong-Myeong;Son, Ho-Sun;Yang, Beon-Seok
    • BMB Reports
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    • 제31권1호
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    • pp.48-52
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    • 1998
  • $p16^{INK4}$, which is a 16-kDa polypeptide protein, inhibits the catalytic activity of the CDK4-cyclinD complex to suppress rumor growth. Both unlabeled and isotope-labeled human tumor suppressor $p16^{INK4}$ protein were overexpressed and purified to characterize biochemical and structural properties. The purified p16 binds to monomeric GST-CDK4 and exists in a monomer conformation for several weeks at $4^{\circ}C$. The circular dichroism (CD) data indicates that p16 contains high percentage of ${\alpha}$-helix and that the helix percentage maximized at pH value of 7.0. One-and two-dimensional nuclear magnetic resonance (NMR) data suggest that purified p16 from our construct has a unique folded conformation under our experimental conditions and exhibits quite stable conformational characteristics.

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Synthesis, Molecular and Microstructural Study of Poly-N-Vinylpyrrolidone Oximo-L-Valyl-Siliconate with IR, 1H-NMR and SEM

  • Singh, Man;Padmaja, G. Vani
    • Bulletin of the Korean Chemical Society
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    • 제31권7호
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    • pp.1869-1874
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    • 2010
  • By reducing PVP with $H_2NOH$.HCl and NaOH 2:2:1 mass ratios in aqueous ethanol, poly-N-vinyl pyrrolidone oxime [PVPO] was prepared with 92% yield. Applying the sol-gel concept, orthosilicic acid [OSA] was made by hydrolyzing TEOS with ethanol in 1:0.5 molar ratios using 1 N KOH aqueous solution as a catalyst. The OSA + PVPO + $_L$-Valine ($\alpha$-amino acid) were mixed with pure ethanolic medium in 1:2:2 mass ratios and refluxed at $78^{\circ}C$ and 6 pH for 6.5 h. A white residue of poly-N-vinyl pyrrolidone oximo-L-valyl-siliconate [POVS] appeared after 5 h. The heating of reaction mixture was stopped and the contents were brought to NTP. The residue formation of POVS was intensified with lowering a temperature and completely solidified within 5 h, was filtered using a vacuum pump with Whatmann filter paper no. 42. The residue of POVS was washed several times with 20% aqueous cold ethanolic solution and dried in vacuum chamber at $25^{\circ}C$ for 24 h. The MP was noted above $350^{\circ}C$. Structural and internal morphology were analyzed with IR and $^1H$-NMR, and SEM respectively. A drug loading and transporting ability of the POVS in water and at pH = 5 and 8 was determined chromatographically.

Spectrophotometric Determination of Allopurinol Drug in Tablets: Spectroscopic Characterization of the Solid CT Complexes

  • Refat, Moamen S.;Mohamed, Gehad G.;Fathi, Ahmed
    • Bulletin of the Korean Chemical Society
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    • 제31권6호
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    • pp.1535-1542
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    • 2010
  • Spectrophotometric micro determination of allopurinol (ALP) via charge-transfer formation is described. This includes the utility of some $\pi$-acceptors such as 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ) and 3,6-dichloro-2,5-dihydroxy-p-benzoquinone (p-CLA) for estimation of ALP drug (act as $\grave{e}$-donor). These reactions are applied for determination of ALP in its pharmaceutical preparations coming from different companies. Elucidation of the chemical structure of the solid CT complexes formed via reaction between drugs under study and $\pi$-acceptors, using elemental analyses (C, H, N), I. R., $^1H$ NMR and mass spectrometry.

Structural Determination of cis- and trans-5-Hydroxymethyl-5-methyl-2-thiono-r-2-ethoxy-1,3,2-dioxaphosphorinane by NMR and X-ray Crystallography: Model Compounds for the Reaction Mechanism Study of Organophosphorus Pesticides

  • Kim, Jeong Han;Toia, Robert F.;Craig, Donald C.
    • Journal of Applied Biological Chemistry
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    • 제43권1호
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    • pp.37-43
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    • 2000
  • 1,3,2-Dioxaphosphorinanes are suitable compounds for studying the stereochemistry of substitution at phosphorus. Cis- and trans-5-hydroxymethl-5-methyl-2-thiono-2ethoxy-1,3,2-dioxaphosphorinane were prepared, and their structures and stereochemistry unambiguously assigned by NMR and X-ray crystallography with acetoxy and 3,5-dinitrobenzoyloxy derivatives, respectively. Trans isomer gave $^{31}P$ NMR signal at higher field than cis isomer, and the ring proton Spectrum of cis isomer showed characteristic pattern for identifying its geometry. In X-ray crystallography they adopted a chair conformation with the ethoxy groups in the axial positions, and the sulfide groups in the equatorial positions. A flattening of the ring around the phosphorus center was noted, the POC bond angles were about $120^{\circ}$, and the C-O bonds in the ring were significantly longer than the C-O bond for the ethoxy group or the C-O bond for hydroxyl group.

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MCM-41, 48 메조포러스 물질 및 SiO2에 담지한 헤테로폴리산의 특성 및 촉매적 활성 (Property and Catalytic Activity of Heteropoly Acid Supported on MCM-41, 48 Mesoporous Material and SiO2)

  • 박정우;김범식;이정민;이관영
    • 공업화학
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    • 제10권7호
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    • pp.1020-1027
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    • 1999
  • 헤테로폴리산(HPW)을 표면적이 서로 다른 담체인 $SiO_2$ MCM-41, MCM-48에 담지농도와 소성온도를 달리하며 담지시켰다. X-선 회절분석, 질소 흡착법, 적외선 흡수 스펙트럼, $^{31}P$ 고체 핵자기 공명을 통해서 이 담지촉매의 특성을 조사하였다. IR과 NMR의 결과로부터 HPW가 담체안에서 케긴 구조를 유지하면서 존재함을 확인할 수 있었다. MCM-41의 경우에는 35 wt %, MCM-48의 경우에는 65 wt %로 담지시킨 경우에도 X-선 회절패턴에서 HPW 고유의 피크가 나타나지 않았으며, 이와 같은 특성을 통해서 HPW가 고분산 되어 있음을 알 수 있었다. Di, bis, tri-pentaerythritol의 가수분해 반응에서 이들 담지 촉매는 높은 촉매 활성을 보였으며 HPW, $HPW/SiO_2$보다 HPW/MCM-41, 48의 촉매 활성이 더 우수하였다.

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