• 제목/요약/키워드: Solution NMR

검색결과 565건 처리시간 0.023초

制癌作用 (STDIES ON ANTITUMOR AGENTS FROM HIGHER PLANTS)

  • Itokawa, Hideji
    • 한국자원식물학회지
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    • 제6권1호
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    • pp.13-23
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    • 1993
  • To data, many types of compounds having antineoplastic activity have been isolated from higher plants, that is, alkalodids, terpenes, lignans, steroids and so on. Some of ther were isolated from Indonesian plants, Curcuma xanthorrhiza and Eurycoma longifolia. Bisaborane type compounds were compounds were isolated as antimeoplastic compounds againest Sarcoma 180A from C. xanthorrhiza, and quassinoids and euryrene type triterpenes from triterpenes from El longifolia. Casearines, a kind of diterpene, had been isolated as cytotxic components from Casearia sylvestris distributed in South America. RA series Cyclic hexapeptides isolated from Rubia akane and R. cordifolia also have strong antineoplastic activity against various types of tumors. Till now, 16 kinds of RA series compounds were isolated and named as RA-I~XVI. Moreover, monoglucoside of RA-V newly isolated from same plant. Many kinds of derivatives including natural RA compounds were tested for QSAR, and one of them, RA-VII was screened up as a most suitable substance as an antitumor agent. RA-VII(=RA 700) has strong cytotoxic activity against KB cells, P388 lymphocytic leukemia and MM2 mammary carcinoma cells. In some solution, three conformers of RA-VII were observed by NMR. It was discussed the relationship between conformation and activity. Total synthesis was already completed, but there is left room for improvement. Phase I clinical trials for RA-VII has been finished, then Phase II trials will be started before long.

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Novel solvothermal approach to hydrophilic nanoparticles of late transition elements and its evaluation by nanoparticle tracking analysis

  • Dutilleul, Marion Collart;Seisenbaeva, Gulaim A.;Kessler, Vadim G.
    • Advances in nano research
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    • 제2권2호
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    • pp.77-88
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    • 2014
  • Solvothermal treatment of late transition metal acetylacetonates in a novel medium composed either of pure acetophenone or acetophenone mixtures with amino alcohols offers a general approach to uniform hydrophilic metal nanoparticles with high crystallinity and low degree of aggregation. Both pure metal and mixed-metal particles can be accesses by this approach. The produced materials have been characterized by SEM-EDS, TEM, FTIR in the solid state and by Nanoparticle Tracking Analysis in solutions. The chemical mechanisms of the reactions producing nanoparticles has been followed by NMR. Carrying out the process in pure acetophenone produces palladium metal, copper metal with minor impurity of $Cu_2O$, and NiO. The synthesis starting from the mixtures of Pd and Ni acetylacetonates with up to 20 mol% of Pd, renders in minor yield the palladium-based metal alloy along with nickel oxide as the major phase. Even the synthesis starting from a mixed solution of $Cu(acac)_2$ and $Ni(acac)_2$ produces oxides as major products. The situation is improved when aminoalcohols such as 2-aminoethanol or 2-dimethylamino propanol are added to the synthesis medium. The particles in this case contain metallic elements and pairs of individual metals (not metal alloys) when produced from mixed precursor solutions in this case.

GMA와 프탈이미드아크릴레이트의 공중합체 합성과 반응성비 (Free-Radical Copolymerization of Glycidyl Methacrylate with Phthalimidoethyl Acrylate : Synthesis and Determination of Monomer Reactivity Ratios)

  • 오승민;오대희
    • 한국응용과학기술학회지
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    • 제30권2호
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    • pp.297-304
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    • 2013
  • Free-radical copolymerization of glycidyl methacrylate(GMA) and N-phthalimidoethyl acrylate(NPEA) were carried out at $60^{\circ}C$ in dimethylformamide(DMF) solution in the presence of benzoylperoxide(BPO) at low conversion. The polymers were characterized by IR and $^1H$-NMR. The compositions of the copolymer was analyzed by ultra violet(UV/Vis) spectrophotometry. The reactivity ratios of the monomer was determined by the application of Fineman-Ross(FR) and Kelen-T$\ddot{u}$d$\ddot{o}$s(KT) methods. The monomer reactivity ratios of the system and Alfrey-Price's resonance effect(Q) and polar effect(e) value for NIEA were determined as follow. The reactivity ratios of the monomer obtained from FR and KT are found to be $r_1$=0.87, $r_2$=0.98 and $r_1$=0.88, $r_2$=0.99 respectively. The Q and e values of poly(GMA-co-NPEM) calculated from $r_1$ and $r_2$ was Q= 1.31, e=0.75 respectively.

Xanthomonas sp. EPS-1이 생산하는 다당류의 리올로지 특성 (Rheological Properties of Exopolysaccharide Produced by Xanthomonas sp. EPS-1)

  • 손봉수;박석규;강신권;이상원;성낙계
    • 한국미생물·생명공학회지
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    • 제23권3호
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    • pp.269-274
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    • 1995
  • For the screening of a new functional exopolysaccharide, sugar composition and rheological properties of exopolysaccharide produced from Xanthomonas sp. EPS-1 were investigated. The average molecular weight of exopolysaccharide was determined to be approximately 2.l $\times$ 10$^{6}$ dalton. The new exopolysaccharide EPS-1 was composed of mannose, glucose, galactose and gluco- samine. IR analysis showed that the exopolysaccharide EPS-1 was assumed to be polymer with carbohydrates. NMR analysis showed that exopolysaccharide EPS-1 was presumed to be 4 units of sugar and trace of CH$_{3}$ group. Exopolysaccharide EPS-1 solution showed a characteristic of non-Newtonian fluid properties. At the concentration of 1.0%, the consistency index and the flow behavior index were shown at 10.8352 poise-sec and 0.4419, respectively. All dispersions were pseudoplastic fluids described accurately by Power-law model. Exopolysaccharide EPS-1 was highly viscous at low concentration, with good stability over a wide range of pH 5 to 13. The excellent compatibility of exopolysaccharide EPS-1 was represented with salts such as sodium chloride.

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Biocompatibility of oxidized alginate/gelatin/BCP -based hydrogel composites

  • Phuong, Nguyen Thi;Min, Young-Ki;Yang, Hun-Mo;Song, Ho-Yeon;Lee, Byong-Teak
    • 한국재료학회:학술대회논문집
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    • 한국재료학회 2010년도 춘계학술발표대회
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    • pp.40.2-40.2
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    • 2010
  • In this study, oxidized alginate/gelatin/biphase calcium phosphate (BCP)- based hydrogel composites were fabricated. Alginate sodium was oxidized by periodate. The oxidized product was confirmed by using $^1H$ and $^{13}C$ NMR spectra. The number average molecular weight ($M_n$), the average molecular weight ($M_w$) of the oxidized alginate were determined by Gel Permeation Chromatography (GPC). The hydrogel was formed from the oxidized alginate and gelatin solution via Schift-base reaction. The hydrogel showed a highly porosity by a Scanning Electron Microscope (SEM) and Mercury Intrusion Porosimetry (MIP). Crosslinked density of the gel matrix were assessd by trinitrobenzene sulfonic acid (TNBS) assay that shows a high effect on swelling ratio. Increment of the crosslinked desity resulted in enhancing compressive strength of the hydrogel composite. The cytotoxity of hydrogel was assessed with osteoblast MG-63. The hydrogel composites show a high compatibility. The obtained results showed a potential application for bone regeneration in future.

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Influence of Quaternization on UCST Properties of Hydroxyl-Derivatized Polymers

  • Lee, Hyung-Il
    • Bulletin of the Korean Chemical Society
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    • 제35권10호
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    • pp.3001-3004
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    • 2014
  • A series of hydroxyl-derivatized quaternized polymers were successfully synthesized by atom transfer radical polymerization (ATRP) and Cu(I)-catalyzed 1,3-dipolar cycloaddition of azide and alkynes (click chemistry), followed by quaternization reactions. ATRP was employed to synthesize poly(2-hydroxyethyl methacrylate) (PHEMA), followed by introduction of alkyne groups using pentynoic acid, leading to HEMA-Alkyne. 2-Azido-1-ethanol and 3-azido-1-propanol were combined with the HEMA-Alkyne backbone via click reaction, resulting in triazole-ring containing hydroxyl-derivatized polymers. Quaternization reactions with methyl iodide were conducted on the triazole ring of each polymer. Molecular weight, molecular weight distribution, and the degree of quaternization (DQ) were determined by gel permeation chromatography (GPC) and $^1H$ NMR spectroscopy. The average molecular weight ($M_n$) of the resulting polymers ranged from $5.9{\times}10^4$ to $1.05{\times}10^5g/mol$ depending on the molecular architecture. The molecular weight distribution was low ($M_w/M_n$ = 1.26-1.38). The transmission spectra of the 0.1 wt % aqueous solutions of the resulting quaternized polymers at 650 nm were measured as a function of temperature. Results showed that the upper critical solution temperature (UCST) could be finely controlled by the level of DQ.

Synthesis of Periodic Mesoporous Organosilica by Microwave Heating

  • Yoon, Sang-Soon;Son, Won-Jin;Biswas, Kalidas;Ahn, Wha-Seung
    • Bulletin of the Korean Chemical Society
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    • 제29권3호
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    • pp.609-614
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    • 2008
  • A periodic mesoporous organosilica material was synthesized by microwave heating (PMO-M) using 1,2-bis(trimethoxysilyl)ethane as a precursor in a cationic surfactant solution, and textural properties were compared with those of the product produced by conventional convection heating (PMO-C). These synthesized materials were characterized using XRD, TEM/SEM, N2 adsorption isotherm, 29Si and 13C NMR, and TGA, which confirmed their good structural orders and clear arrangements of uniform 3D-channels. Synthesis time was reduced from 21 h in PMO-C to 2-4 h in PMO-M. PMO-M was made of spherical particles of 1.5-2.2 m m size, whereas PMO-C was made of decaoctahedron-shaped particles of ca. 8.0 m m size. Effect of synthesis temperature, time, and heating mode on the PMO particle morphology was examined. The particle size of PMO-M could be controlled by changing the heating rate by adjusting microwave power level. PMO-M demonstrated improved separation of selected organic compounds compared to PMO-C in a reversed phase HPLC experiment. Ti-grafted PMO-M also resulted in higher conversion in liquid phase cyclohexene epoxidation than by Ti-PMO-C.

바나듐 (v)-아미노폴리카르본산 착물의 탄소-13 및 바나듐-51 핵자기공명연구 (제1보) (Carbon-13 and Vanadium-51 Nuclear Magnetic Resonance Studies of Vanadium(v)-Aminopolycarboxylic Acids (Ⅰ))

  • 이만호;오대섭
    • 대한화학회지
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    • 제27권2호
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    • pp.117-126
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    • 1983
  • 탄소-13 및 바나듐-51 핵자기공명분광법을 이용하여 아미노폴리카르본산-바나듐(v) 착물의 용액 내에서의 구조에 대해 연구하였다. 이 때 사용한 리간드는 ethylenediaminetetraacetic acid (EDTA), trans-cyclohexanediaminetetraacetic acid (CDTA), 1,2-propylenediaminetetraacetic acid (PDTA), ethylenediaminediacetic acid (EDDA), 2-hydroxyethylethylenediaminetriacetic acid (HEDTA), diethylenetriaminepentacetic acid (DPTA), nitrilotriacetic acid (NTA) 등이었다. 모든 리간드는 바나듐(Ⅴ)과 시스-VO2핵을 함유하는 정8면체 구조의 1:1 착물을 생성하였다. 바나듐(V)과 시스-$VO_2$ 핵을 함유하는 정8면체 구조의 1:1 착물을 생성하였다. 바나듐(V)에 대한 히드록시에틸기의 배위는 아세테이트기의 배위에 비해 덜 바람직함을 알 수 있었다. 그리고 EDDA 및 PDTA는 각각 2가지의 이성체착물들을 생성함을 알 수 있었다.

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A Study on the Copolymerization Kinetics of Phenylethyl Acrylate and Phenylethyl Methacrylate

  • Lee, Han-Na;Tae, Gi-Yoong;Kim, Young-Ha
    • Macromolecular Research
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    • 제16권7호
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    • pp.614-619
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    • 2008
  • Copolymers of phenyl alkyl acrylates/methacrylates are used clinically as soft materials for the foldable intraocular lens (IOL) to treat cataracts. In this study, copolymers of 2-phenylethyl acrylate (PEA) and 2-phenylethyl methacrylate (PEMA) of various compositions were prepared using free radical polymerization in solution. The composition of the copolymers was determined by $^1H$-NMR analysis. The reactivity ratios of the monomers were calculated using the conventional Fineman-Ross or Kelen-Tudos method. The reactivity ratio of PEA ($r_1$) and PEMA ($r_2$) were estimated to be 0.280 and 2.085 using the Kelen-Tudos method, respectively. These values suggest that PEMA is more reactive in copolymerization than PEA, and the copolymers will have a higher content of PEMA units. The glass transition temperature ($T_g$) of the copolymers increased with increasing PEMA content. The molecular weight and polydispersity indices ($M_w/M_n$) of the polymers were determined by GPC. Overall, these results are expected to be quite useful in applications to foldable soft IOL materials.

Backbone 1H, 15N, and 13C Resonance Assignments and Secondary-Structure of Conserved Hypothetical Protein HP0894 from Helicobacter pylori

  • Han, Kyung-Doo;Park, Sung-Jean;Lee, Bong-Jin
    • Molecules and Cells
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    • 제20권3호
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    • pp.442-445
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    • 2005
  • HP0894 (SwissProt/TrEMBL ID O25554) is an 88-residue conserved hypothetical protein from Helicobacter pylori strain 26695 with a calculated pI of 8.5 and a molecular weight of 10.38 kDa. Proteins with sequence similarity to HP0894 exist in Vibrio choierae, Enterococcus faecalis, Campylobacter jejuni, Streptococcus pneumoniae, Haemophilus influenzae, Escherichia coli O157, etc. Here we report the sequence-specific backbone resonance assignments of HP0894. About 97.5% (418/429) of the HN, N, CO, $C{\alpha}$, $C{\beta}$ resonances of the 88 residues of HP0894 were assigned. On the basis of these assignments, three helical regions and four strand regions were identified using the CSI program. This study is a prerequisite for calculating the solution structure of HP0894, and studying its interaction with its substrates, if any, and/or with other proteins.