• Title/Summary/Keyword: $^{31}P$ NMR spectroscopy

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The Effect of Gingko Biloba Extract on Energy Metabolic Status in C3H Mouse Fibrosarcoma : Evaluated by in vivo $^{31}P$ Magnetic Resonance Spectroscopy (Gingko biloba extract가 C3H 마우스 섬유육종의 에너지 대사 상태에 미치는 영향 : 생체내 $^{31}P$ 자기공명 분광법을 이용한 분석)

  • Ha Sung Whan;Kim Won Dong;Ahn Yong Chan;Park Chan Il;Lim Tae Hwan;Lee Tae Kuen
    • Radiation Oncology Journal
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    • v.20 no.2
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    • pp.147-154
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    • 2002
  • Purpose : Gingko biloba extract (GBE), a natural product extracted from Gingko leaves, is known to increase the radiosensitivity of tumors. This radiosensitization probably arises from the increase in the peripheral blood flow by decreasing the blood viscosity and relaxing the vasospasm. The influence of a GBE on the metabolic status in fibrosarcoma II (FSall) of a C3H mouse was investigated using $^{31}P$ magnetic resonance spectroscopy (MRS). Materials and Methods : Eighteen C3H mice with fibrosarcoma II $(from\;100\;mm^3\;to\;130\;mm^3)$ were prepared for this experiment. The mice were divided into 2 groups; one (9 mice) without a priming dose, and the other (9 mice) with a priming dose of GBE. The GBE priming dose (100 mg/kg) was administered by an intraperitoneal (i.p.) injection 24 hours prior to the measurement. First $^{31}P$ MRS spectra were measured in the mice from each group as a baseline and test dose of GBE (100 mg/kg) was then administered to each group. One hour later, the $^{31}P$ MRS spectra were measured again to evaluate the change in the energy metabolic status. Results : In the group without the priming dose, the mean pH, PCr/Pi, PME/ATP, Pi/ATP, PCr/(Pi+PME) values 1 hour after the test dose were not changed significantly compared to the values at the baseline. However, in the group with the priming dose, the mean PCr/Pi, Pi/ATP, PCr/(Pi+PME) values 1 hour after the test dose changed from the baseline values of 0.49, 0.77, 0.17 to 0.74, 0.57, 0.28 respectively. According to the paired t-test, the differences were statistically significant. Conclusion : The above findings suggest that the metabolic status is significantly improved after administering GBE if the priming dose is given 24 hours earlier. This shows that the radiosensitizing effect of GBE is based on the increase of tumor blood flow and the improvement in the metabolic status.

Synthesis and Configurational Analysis of Diastereomers of $5^{\prime}-O-(2^{\prime}-Deoxyadenosyl)-3^{\prime}-O-(2^{\prime}$-deoxyadenosyl)-Phosphorothioate

  • Byung Jo Moon;Kyung Lan Huh;Sang Kook Kim
    • Bulletin of the Korean Chemical Society
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    • v.14 no.1
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    • pp.52-55
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    • 1993
  • A procedure is described for the synthesis of the title compound via phosphotriester intermediates. The preparation of $R_p\;and\;S_p$ diastereomeric dinucleotide of d[Ap(S)A] was performed by the condensation of protected deoxyadenosine, 2,5-dichlorophenylphosphorodichloridothioate and 1-hydroxybenzotriazole in THF. Their designation of configuration at phosphorus as $R_p\;and\;S_p$ follows from analysis of $^{31}P$-NMR spectroscopy and reversed-phase HPLC and the stereospecificity in the hydrolysis catalyzed by nuclease Pl.

The Effect of Ginkgo Biloba Extract on Hypoxic Fraction of C3H Mouse Fibrosarcoma (Ginkgo Biloba Extract가 C3H 마우스 섬유육종의 저산소세포 분획에 미치는 영향)

  • Cho Chul Koo;Yi Chun Ja;Ha Sung Whan;Park Charn Il
    • Radiation Oncology Journal
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    • v.13 no.3
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    • pp.205-214
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    • 1995
  • Purpose : To investigate the effect of Ginkgo biloba extract (GBE) on hypoxic cell fraction and metabolic status in fibrosarcoma (FSa II) of C3H mouse. Materials and Methods : Fibrosarcoma (FSa II) 6 mm in diameter, growing in the right hindleg muscle of C3H mouse was used for estimation of hypoxic cell fraction using comparison of $TCD_{50}$. Radiation was given one hour after administration of GBE (100 mg/kg. i.p.) with or without priming dose of GBE (100 mg/kg, i.p.) given 24 hours earlier. Radiation was also given under air breathing condition or clamp hypoxia without GBE as controls. $^{31}p$ NMR spectroscopy was performed before and one hour after administration of GBE with or without priming dose of GBE. Results : $TCD_{50/120's}$ were 81.7 (77.7-86.0) Gy when irradiated under clamped hypoxia 69.6 (66.8-72.5) Gy under air breathing condition. 67.5 (64.1-71.1) Gy with a single dose of GBE (100 mg/kg) given one hour before irradiation, and 62.2 (59.1-65.5) Gy with two doses of GBE given at 25 hours and one hour before irradiation. The hypoxic cell fractions, estimated from $TCD_{50/120's}$, were $10.6{\%}$ under air breathing condition, $7.2{\%}$ after a single dose of GBE, and $2.7{\%}$ after two doses of GBE. The results of $^{31}P$ NMR spectroscopy were as follow. PCr/Pi ratio was $0.27{\pm}0.04$ and $0.40{\pm}0.04$ before and one hour after a single dose of GBE (p<0.05), respectively, without priming dose and $0.30{\pm}0.02$ and $0.71{\pm}0.04$, respectively, with priming dose (p<0.01). These findings indicate that the metabolic status is slightly improved after a single dose and markedly after repeated administrations. Conclusion : GBE decreases the hypoxic cell fraction and imprvoes the meta bolic status of tumor, probably by increasing the blood flow and delivery of oxygen and nutrients, resulting in increased radiosensitivity of tumor.

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

  • Park, Jung-Woo;Kim, Beom-Sik;Lee, Jung-Min;Lee, Kwan-Young
    • Applied Chemistry for Engineering
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    • v.10 no.7
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    • pp.1020-1027
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    • 1999
  • Heteropoly acid(HPW) catalysts supported on three different carriers, an amorphous silica, MCM-41 and MCM-48, with different loadings and calcination temperatures have been prepared and characterized by X-ray diffraction, nitrogen physorption, infrared spectroscopy, and $^{31}P$ magic angle spinning NMR. From the result of IR and NMR, it was shown that HPW retains the Keggin structure on the supported catalysts. No HPW crystal phase was developed even at HPW loadings as high as 35 wt % on the MCM-41 and 65 wt % MCM-48. Thus, HPW appeared to form finely dispersed species. In the hydrolysis reaction of di, bis, tri-pentaerythritol, HPW/MCM-41, 48 exhibited higher catalytic activity than $HPW/SiO_2$ or HPW.

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$[Ni(dppe)_2]$의 합성 및 구조 (Synthesis and Structure of $[Ni(dppe)_2] (dppe=Ph_2PCH_2CH_2PPh_2)$)

  • Kim, Wan -Sung;Lee, Ji-Hwa;Lee, Soon W.
    • Korean Journal of Crystallography
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    • v.11 no.2
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    • pp.80-83
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    • 2000
  • Compound [Ni(P(OEt)3)4] (1) reacted with bis(diphenylphosphino)ethane (Ph2PCH2CH2Ph2, dppe) to give bis(bis(diphenylphosphine)ethane)nickel(0), [Ni(dppe)2] (2). Compound 2 was characterized by spectroscopy (1H-and 31P{1H}-NMR) and X-ray crystallography. Crystallographic data for 2: monoclinic space group P21/n, a=9.826(1)Å, b=21.167(2)Å, c=21.425(2)Å, β=91.957(9)°, Z=4, R(wR2)=0.0377(0.0882).

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Synthesis and Antibacterial Evaluation of Some Novel 2-Arylamino-4-phenyl-thiazolyl Derivatives

  • Parmar, Kokila A.;Suthar, Bharat G.;Parajapati, Sarju
    • Bulletin of the Korean Chemical Society
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    • v.31 no.4
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    • pp.793-797
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    • 2010
  • A series of 2-aminothiazoles derivatives have been synthesized and tested for in vitro antibacterial activity on different microorganisms. Syntheses have been carried out following simple methodology in excellent isolated yields. The structure and purity of the original compounds were confirmed by IR, NMR, Mass spectroscopy, and elemental analysis. All compounds were tested for antibacterial activity against S. aureus, S. pyogenes, E. coli, P. aeruginosa, S. typhi and V. parahaemolyticus. These preliminary results indicate that some of compounds are exhibiting good activity.

FUNGAL EXTRACELLULAR POLYSACCHARIDES INVOLVED IN RECYCLING OF METABOLITES AND OSMOTOLERANCE OF PENICILLIUM FELLUTANUM : APPLICATION OF $^{13}$ C-NMR SPECTROSCOPY FOR THE STUDY ON FUNGAL PHYSIOLOGY AND METABOLISM

  • Park, Yong-Il;Gander, John.-E.
    • Proceedings of the Korean Society for Applied Microbiology Conference
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    • 2000.04a
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    • pp.208-213
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    • 2000
  • Penicillium fellutanum produces a phosphorylated, choline-containing extracellular peptido-polysaccharide, peptidophosphogalactomannan (pPxGM) (8). The $\^$13/C-methyl labeled pPxGM ([methyl-$\^$13/C]pPxGM) was prepared from the cultures supplemented with L-[methyl-$\^$13/C]methionine or [2-$\^$13/C]glycine and was used as a probe to monitor the fate of phosphocholine in this polymer. Addition of purified [methyl-$\^$l3/C]pPxGM to growing cultures in low phosphate medium resulted in the disappearance of [methyl-$\^$13/C]phosphocholine and -N,N'-dimethyl-phosphoethanolamine from the added [methyl-$\^$13/C]pPxGM. Two $\^$l3/C-methyl-enriched cytoplasmic solutes, choline-O-sulfate and glycine betaine, were found in mycelial extracts, suggesting that phosphocholine-containing extracellular pPxGM of P.fellutanum is a precursor of intracellular choline-O-sulfate and glycine betaine and thus of phosphatydilcholine (l0). $\^$13/C-Methyl-labeled cells grown in 3 M NaCl-containing medium showed 2.6- and 22-fold more accumulation of $\^$13/C-methyl labeled choline-O-sulfate and glycine betaine, respectively, originated from the extracellular [$\^$13/C-methyl]pPxGM than those grown without added NaCl. The results suggest that, in addition to glycerol and erythritol, glycine betaine and choline-O-sulfate and thus choline are also osmoprotectants and hence that pPxGM is involved in osmotolerance of this fungus (11). Taken collectively, the $\^$l3/C- and $\^$31/P-NMR analyses of cytosolic solute pools and structural modulation of extracellular pPxGM corresponding to environmental stimuli in P. fellutanum, provided evidence that pPxGM is involved in cellular choline metabolism, osmotolerance, and recycling of metabolites.

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Syntheses and Theoretical Study of Palladium(II) Complexes with Aminophosphines as 7-Membered Chelate Rings

  • 김봉곤;양기열;정맹준;이배욱;도명기
    • Bulletin of the Korean Chemical Society
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    • v.18 no.11
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    • pp.1162-1166
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    • 1997
  • Nature of palladium(Ⅱ) complexes with 7-membered chelates was studied by experimental and theoretical methods on a Pd(L)Cl2 system, where L is Ph2PNHCH2CH2NHPPh2(L1), Ph2PNHC6H4NHPPh2(L2). The palladium(Ⅱ) complexes were prepared and characterized by elemental analysis, IR, UV, 1H, and 31P NMR spectroscopy. Ab initio calculations with geometry optimizations were also performed for related model systems, Pd(L)Cl2; L=R2PNH(CH2)2NHPR2(L3), R2PNHC6H4NHPR2(L4), R2P(CH2)4PR2(L5), R2PCH2(C6H4)CH2PR2(L6); R=H, CH3.

Photoreactivity of $ReH_5$(Cyttp) (Cyttp=Php$(CH_2CH_2CH_2PCy_2)_2)$ with CO, $CO_2\;and\;PMe_3$

  • Lee, Myung-Young;Shin, Dae-Ho;Kim, You-Hyuk
    • Bulletin of the Korean Chemical Society
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    • v.15 no.7
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    • pp.571-576
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    • 1994
  • The photoreactions of $ReH_5(Cyttp)\;(1)\;(Cyttp=PhP(CH_2CH_2CH_2PCy_2)_2)\;with\;CO,\;CO_2\;and\;PMe_3 has been investigated to find the differences in reactivities from those of trismonophosphine analog. Irradiation of 1 under CO, $CO_2$ and excess $PMe_3$ in benzene results in the formation of the complexes, $ReH(CO)_2(Cyttp)\;(2),\;ReH_2({\eta}^2-HCO_2)(Cyttp)\;(3)\;and\;$ReH_3(PMe_3)(Cyttp)$ (4), respectively. The resulting products suggest that photoreactions of $ReH_5(Cyttp)$ proceed by photoextrusion of $H_2$ giving a phototransient species "$ReH_3$(Cyttp)" which can be trapped by CO, $CO_2\;and\;PMe_3$. The structures of 2, 3 and 4 are inferred based on $^1H,\;^{31}P$ NMR and I. R spectroscopy.

Cycloplatinated Complexes of Thiosemicarbazones. Synthesis and Crystal Structure of [$Ph_2PC_6H_4CHNNC(S)NHCH_3PtCl$]

  • 유동원;강상욱;고재정;최문근
    • Bulletin of the Korean Chemical Society
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    • v.18 no.3
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    • pp.305-310
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    • 1997
  • The synthesis and characterization of the platinum heterocyclic carboxaldehyde thiosemicarbazone complexes [NC5H4CRNNC(S)NHR'PtCl] (R=H, R'=CH3(1); R=CH3, R'=CH3(2); R=CH3, R=H(3)) and diphenylphosphinophenyl carboxaldehyde thiosemicarbazone complexes [Ph2PC6H4CHNNC(S)NHRPtCl] (R=CH3(5); R=iC3H7(6); R=Ph(7)) are described. Compounds 1-3 were prepared by reaction of Pt(SEt2)2Cl2 with 2-acetylpyridine-4-alkylthiosemicarbazone in the presence of NEt3. Compounds 5-7 were prepared using Pt(SEt2)2Cl2 in toluene with diphenylphosphinophenyl carboxaldehyde alkylthiosemicarbazone. The compounds have been characterized by microanalysis, NMR (1H, 13C, 31P) spectroscopy, and single-crystal X-ray diffraction. X-ray single crystal diffraction analysis reveals that compound 5 is a mononuclear platinum compound with P,N,S-coordination mode.