• Title/Summary/Keyword: $^{1}H$ NMR

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Extraction and Bioassay of Allelochemicals in Jerusalem Artichoke

  • Sungwook Chae;Lee, Ho-Jin
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.46 no.4
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    • pp.309-316
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    • 2001
  • Helianthus tuberosus has been known to inhibit the growth of weeds and other plants sharing its habitat. This study was conducted to identify the allelochemicals of Helianthus tuberosus which were extracted with water and solvents. Aqueous extracts of leaf, stem, root, tuber and tuber peel of Helianthus tuberosus except tuber did not show significant differences in phytotoxicity to alfalfa seedlings. It was considered that Helianthus tuberosus contained fewer or less potential water-soluble substances that were toxic to alfalfa. Methanol extract of leaves of Helianthus tuberosus was sequentially partitioned in increasing polarity with n-hexane, ethylacetate and n-butanol. Each extract had a yield of 148, 12, 15.7 and 9.5g, respectively. Inhibitory effects on germination of alfalfa seeds treated with four fractions were not significantly different. But the significant reductions on hypocotyl length were observed for all the solvent extracts. Among the four fractions, the ethylacetate fraction showed the most significant inhibition effect on bioassay with alfalfa. Further separation of the active ethylacetate fraction by open column chromatography led to the 25 subfractions. In bioassay of each sub-fraction with alfalfa seeds, sub-fraction No. 13 showed the most inhibitory effect on seedling growth. $^1$H NMR and gas chromatography-mass spectrometry analysis revealed that sub-fraction No. 13 was the mixture of straight-chain saturated fatty acids.

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Trifunctional Amino Acid-Co(III) Complexes of N,N'-Dimethylethylenediamine-N,N'-di-${\alpha}$-butyric Acid (N,N'-Dimethylethylenediamine-N,N'-di-${\alpha}$-butyric acid 의 세자리 리간드 아미노산 코발트 (III) 착물)

  • Moo Jin Jun;Chung Hae Kwon;Jin Seung Jung
    • Journal of the Korean Chemical Society
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    • v.33 no.5
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    • pp.504-509
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    • 1989
  • Cobalt(III) complexes of N,N'-dimethylethylenediamine-N,N'-di-${\alpha}$-butyric acid(dmedba) and trifunctional aminoacids, [Co(dmedba)(L-aa)] (L-aa = S-methyl-L-cysteine, L-methionine, L-glutamic acid, L-aspartic acid) have been prepared from the reaction between the $ s-cis-[Co(dmedba)Cl_2]-^$ complex and the amino acid. The amino acids have been found to coordinate through the amine and carboxylate groups just like [Co(dmedda)(L-aa)]. The complexes obtained in this work were characterized by their proton magnetic resonance, infrared and visible absorption spectral data along with the elemental analyses.

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Methotrexate-Incorporated Polymeric Micelles Composed of Methoxy Poly(ethylene glycol)-Grafted Chitosan

  • Jeong, Young-Il;Seo, Dong-Hyuk;Kim, Don-Gon;Choi, Chang-Yong;Jang, Mi-Kyeong;Nah, Jae-Woon;Park, Yoon-Kyung
    • Macromolecular Research
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    • v.17 no.7
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    • pp.538-543
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    • 2009
  • In this study, methotrexate (MTX)-encapsulated polymeric micelles using methoxy poly(ethylene glycol) (MPEG)-grafted chitosan (ChitoPEG) copolymer were prepared. The MIX-incorporated polymeric micelles of ChitoPEG copolymer has a particle size of around 50-100 nm. In 1H nuclear magnetic resonance (NMR) study, the specific peaks of MTX disappeared in heavy water ($D_2O$) and only the specific peak of MPEG was observed, while all of the peaks were confirmed in dimethyl sulfoxide (DMSO). These results indicated that MTX was complexed with chitosan and then formed an ion complex inner-core of the polymeric micelle in an aqueous environment. The drug contents of the polymeric micelle were around $4{\sim}12%$ and the loading efficiency of MTX in the polymeric micelles was higher than 60% (w/w) for all of the formulations. The cytotoxicity of MIX and MTX-incorporated polymeric micelle against CT26 tumor cells was not significantly changed.

Synthesis and Characterization of Sulfonated Poly(arylene ether) Polyimide Multiblock Copolymers for Proton Exchange Membranes

  • Lee, Hae-Seung;Roy Abhishek;Badami Anand S.;McGrath James E.
    • Macromolecular Research
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    • v.15 no.2
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    • pp.160-166
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    • 2007
  • Novel multiblock copolymers, based on segmented sulfonated hydrophilic-hydrophobic blocks, were synthesized and investigated for their application as proton exchange membranes. A series of segmented sulfonated poly(arylene ether sulfone)-b-polyimide multiblock copolymers, with various block lengths, were synthesized via the coupling reaction between the terminal amine moieties on the hydrophilic blocks and naphthalene anhydride functionalized hydrophobic blocks. Successful imidization reactions required a mixed solvent system, comprised of NMP and m-cresol, in the presence of catalysts. Proton conductivity measurements revealed that the proton conductivity improved with increasing hydrophilic and hydrophobic block lengths. The morphological structure of the multiblock copolymers was investigated using tapping mode atomic force microscopy (TM-AFM). The AFM images of the copolymers demonstrated well-defined nanophase separated morphologies, with the changes in the block length having a pronounced effect on the phase separated morphologies of the system. The self diffusion coefficient of water, as measured by $^1H$ NMR, provided a better understanding of the transport process. Thus, the block copolymers showed higher values than Nafion, and comparable proton conductivities in liquid water, as well as under partially hydrated conditions at $80^{\circ}C$. The new materials are strong candidates for use in PEM systems.

Identification of Phytotoxins Produced by Drechslera portulacae, a Pathogen of Purslane(Portulaca oleracea) - II. Isolation of Zeaenol and Its Herbicidal Activity (쇠비름(Porturaca oleracea)의 병원균, Drechslera portulacae가 생산하는 식물독소의 구조 동정 - 제 2 보. Zeaenol의 단리 및 제초활성)

  • Kim, K.W.
    • Korean Journal of Weed Science
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    • v.14 no.3
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    • pp.192-198
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    • 1994
  • Zeaenol isolated from the culture filtrate of a fungal weed pathogen Drechslera portulacae, which causes necrosis on the leaves and stem of purslane (Portulaca oleracea). Its structure was determined by single-crystal x-ray diffraction method together with assignments of $^1H$ and $^{13}C$-NMR experiments. Zeaenol inhibited root length of Echinochloa crus-galli and Abutilon avicennae by 22.8% and 54.8% at $3{\times}10^{-6}M$, respectively.

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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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    • v.20 no.3
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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.

The Feasibility Study of 3-D Magnetic Resonance Neurograms (자기공명단층촬영장치를 이용한 신경조영영상의 기초연구)

  • Mun, C.W.;Lee, S.Y.;Lim, T.H.
    • Proceedings of the KOSOMBE Conference
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    • v.1993 no.05
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    • pp.28-30
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    • 1993
  • We have investigated the feasibility study, especially for optimal TR, to obtain 3-D MR neurographic imaging (neurograms or nervography) which shows the distribution of peripheral nerve fibers at the human forearm using 4.7 T magnet. To peform a successful formation of MR neurographic imaging, nerve signal should be separated from the other signal comes from surrounding muscle or fat, because nerves are usually embeded in muscle or fat. Generally, it is well known that nerve has shoter T1 value than that of muscle. Thus, repetition time was optimized to maximize the signal intensity defference between the muscel and nerve. We have also used spin-echo(SE) sequence with long echo time($60{\sim}90\;msec$) to enhance the different signal intensity between muscles and pheriperal nerves base on the fact that muscle tissue has longer T2 relaxation lime than that or nerve.

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Chelation of Calcium Ions by Poly(${\gamma}$-Glutamic Acid) from Bacillus subtilis (Chungkookjang)

  • Tsujimoto, Takashi;Kimura, Junya;Takeuchi, Yasushi;Uyama, Hiroshi;Park, Chung;Sung, Moon-Hee
    • Journal of Microbiology and Biotechnology
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    • v.20 no.10
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    • pp.1436-1439
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    • 2010
  • Many studies have clarified that poly(${\gamma}$-glutamic acid) (PGA) increases the solubility of $Ca^{2+}$, suggesting that PGA enhances calcium absorption in the small intestine. However, there has been no report on the specific interaction between PGA and $Ca^{2+}$ in water. We studied the aqueous solution properties of PGA calcium salt (PGA-Ca complex). The chelating ability and binding strength of PGA for $Ca^{2+}$ were evaluated. The PGA-Ca complex was soluble in water, in contrast to the insolubility of poly(acrylic acid) (PAA) calcium salt, and the chelating ability of PGA for $Ca^{2+}$ was almost the same as that of PAA. The globular conformation of the PGA-Ca complex in water was estimated by SEC and viscosity measurements. The chelation ability of PGA for $Ca^{2+}$ was examined by $^1H$ NMR. The present study showing the characteristics of the PGA-Ca complex will provide useful information about the calcium absorption by PGA in vivo.

Design and decoration of heparin on porous nanosilica via reversible disulfide linkages for controlled drug release

  • Nguyen, Dai Hai
    • Journal of IKEEE
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    • v.21 no.3
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    • pp.320-330
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    • 2017
  • Porous nanosilica (PNS) has been identified as a potential candidate for controlled drug delivery. However, unmodified PNS-based carriers exhibited an initial release of loaded bioactive agents, which may limit their potential clinical applications. In this study, the surface of PNS was functionalized with adamantylamine (ADA) via disulfide bonds (-S-S-), PNS-S-S-ADA, which was then modified with cyclodextrin (CD)-heparin (Hep) (CD-Hep), PNS-S-S-CDH, for redox triggered rhodamine B (RhB) delivery. The obtained samples were then characterized by proton nuclear magnetic resonance ($^{1}H\;NMR$), Fourier transform infrared (FTIR), and transmission electron microscope (TEM). These results showed that PNS-S-S-CDH was successfully formed with spherical shape and average diameter of $45.64{\pm}2.33nm$. In addition, RhB was relatively encapsulated in the PNS-S-S-CDH (RhB@PNS-S-S-CDH) and slowly released up to 3 days. The release of RhB, in particular, was triggered due to the cleavage of -S-S- in the presence of dithiothreitol (DTT). It might be anticipated that the modified PNS can be used as redox-responsive drug delivery system in cancer therapy.

Bulk Coordination Polymerization of Dicyclopentadiene (DCPD) by Pd Complexes Containing β-Ketoiminate or β-Diketiminate Ligands

  • Lee, Eung Jun;Kim, Ho Sup;Lee, Byoung Ki;Hwang, Woon Sung;Sung, Ik Kyoung;Lee, Ik Mo
    • Bulletin of the Korean Chemical Society
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    • v.33 no.12
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    • pp.4131-4136
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    • 2012
  • Several palladium complexes containing ${\beta}$-ketoiminate and ${\beta}$-diketiminate ligands successfully produced poly(DCPD) possibly via vinyl addition. It was found that catalysts with ${\beta}$-diketiminate ligands containing bulkier aryl substituents showed the highest activity in the presence of MAO as a cocatalyst. Purity of DCPD is quite essential for the higher activity and small amount of organic solvent such as $CH_2Cl_2$ and toluene is required to reduce the viscosity of the reactant mixture for the higher activity. $^1H$ NMR spectra of produced polymers with N,N-dimethylanilinium tetra(pentafluorophenyl)borate (N,N-DAPFAr"$_4$) show that 5,6-double bond of DCPD is removed with 2,3-double bond remaining. Produced poly(DCPD) with MAO cocatalyst is quite rigid and insoluble in common organic solvents but rather brittle.