• Title/Summary/Keyword: NMR study

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Study on preparation and characterization of PPV LB films. (Poly(p-phenylenevinylene) (PPV) LB 막의 제작 및 특성 연구)

  • Kim, J.H.;Kim, K.S.;Kang, W.H.;Sohn, M.H.;Kim, Y.C.;Kim, Y.K.;Sohn, B.C.
    • Proceedings of the KIEE Conference
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    • 1994.11a
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    • pp.219-221
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    • 1994
  • Oil-soluble poly(p-phenylene(1-methoxyethylene)), as a precursor of poly(p-phenylenevinylene) (PPV), was synthesized add identified with NMR and FT-IR spectroscopy. The PPV films were prepared by PPV precursor films with a thermal treatment at $250^{\circ}C$ under vacuum, where the PPV precursor films wets formed on various substrates by using Langmuir-Blodgett(LB) method. The characterization of these films was carried out by FT-IR spectroscopy, UV-VIS absorption spectroscopym, and photoluminescence (PL). Atomic Force Microscopy (AFM) has been used to investigate He surface morphology of PPV films.

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Synthesis and Antitumor Activity of Phthalimide-Based Polymers Containing Camptothecin

  • Lee, Neung-Ju
    • Macromolecular Research
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    • v.11 no.1
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    • pp.47-52
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    • 2003
  • The objective of this study was to develop a polymeric drug delivery system for camptothecin (CPT), capable of improving its therapeutic index and reducing its side effects. A monomeric conjugate, 3,6-endo-methylene-1,2,3,6-tetrahydrophthalimidoethanoylcamptothecin in (ETECPT) between CPT and 3,6-endo-methylene-1,2,3,6-tetrahydrophthalimidoethanoic acid was synthesized. Its homo-and copolymer with acrylic acid (AA) were prepared by photopolymerization using 2,2-dimethoxy-2-phenylacetophenone (DMP) as a photoinitiator. The monomer and its polymers were characterized by IR, $^1$H- and $^{13}$ C-NMR spectra. The ETECPT content in poly(ETECPT-co-AA) obtained by elemental analysis was 82 wt%. The number-average molecular weights of the polymers determined by gel permeation chromatography were as follows: M$_{n}$ = 11,400 for poly(ETECPT), M$_{n}$ = 17,900 for poly(ETECPT-co-AA). The $IC_{50}$/ values of ETECPT and its polymers against cancer cells were much larger than that of CPT. Our results from the in vivo antitumor activity indicated that all polymers show high antitumor activity than CPT at a dose of 100 mg/kg./kg.

Synthesis of New pH-Sensitive Amphiphilic Block Copolymers and Study for the Micellization Using a Fluorescence Probe

  • Kim, Kyung-Min;Choi, Song-Yee;Jeon, Hee-Jeong;Lee, Jae-Yeol;Choo, Dong-Joon;Kim, Jung-Ahn;Kang, Yong-Soo;Yoo, Hyun-Oh
    • Macromolecular Research
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    • v.16 no.2
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    • pp.169-177
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    • 2008
  • This paper reports a facile synthesis of new water-soluble poly(ethylene oxide) (PEO)-based amphiphilic block copolymers showing pH sensitive phase transition behaviors. The copolymers were prepared by atom transfer radical polymerization (ATRP) of methacrylamide type of monomers carrying a sulfonamide group using a PEO-based macroinitiator and a Cu(I)Br/$Me_6TREN$ catalytic system in aqueous media. The resulting polymers were characterized by a combination of $^1H$-NMR, size exclusion chromatography, and UV/Visible spectrophotometeric analysis. The micellization of the block copolymers as a drug-loading mechanism in aqueous media using fluorescein salt was examined as a function of pH. The stable micelle formation and its loading efficacy suggest that the block copolymers can be used as precursors for drug-nanocontainers.

Preparation and Characterization of Self-aggregated Nanoparticles of Chitosan-Lipoic Acid Conjugate (키토산-리포산 자기 조립체의 제조 및 특성)

  • Park, Eun-Ju;Kim, Young-Jin
    • Polymer(Korea)
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    • v.32 no.6
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    • pp.544-548
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    • 2008
  • The objective of this study is to obtain the anti-oxidant nanoparticles based on biocompatible polymers. It was chosen to conjugate with chitosan as the biodegradable polymer and lipoic acid as the hydrophobic anti-oxidant. Lipoic acid helps the regeneration of exogenous and endogenous anti-oxidants vitamin as well as glutathione and hence acts as antioxidant indirectly. Chitosan was prepared from chitin which was deacetylated under alkali solution for the various reaction time. Lipoic acid-chitosan complex was confirmed by $^1H$-NMR. The critical aggregation concentration was measured using pyrene and the values were about $5{\times}10^{-3}$ g/L. The particle shapes and sizes of the chitosan-lipoic acid nano-particles were about 135 nm that measured by DLS and TEM.

Changes of Antioxidant Activity and Ingredient in Medicinal Plants by Processing (수치에 의한 생약의 항산화 활성 및 성분 변화)

  • Cha, Bae-Cheon;Jun, Kyung-Su
    • Korean Journal of Pharmacognosy
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    • v.43 no.1
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    • pp.46-53
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    • 2012
  • This study was conducted to investigate the change of antioxidant activity and ingredient in 4 species medicinal plant by processing. As a result, EtOAc extract and n-BuOH extract obtained from Cistanche deserticola Y. C. Ma and processed Cistanche deserticola Y. C. Ma showed difference on the experiment of antioxidant activity by DPPH method. Change of ingredient also was confirmed by TLC and HPLC analyses. Two main compounds of antioxidant activity change were isolated by column chromatography from the EtOAc extract and n-BuOH extract of Cistanche deserticola Y. C. Ma. The chemical structure of the compound 1 isolated from EtOAc extract of Cistanche deserticola Y. C. Ma was elucidated as 2'-acetylacteoside by means of IR and NMR analyses. Also, the chemical structure of the compound 2 isolated from n-BuOH extract of Cistanche deserticola Y. C. Ma was confirmed as acteoside. The antioxidant activity of processed Cistanche deserticola Y. C. Ma. was declined by 3 time decrements of 2'-acetylacteoside such as 1.89 mg/g to 0.62 mg/g and 2 time decrements of acteoside such as 5.81 mg/g to 2.67 mg/g by processing.

[ $CO_2$ ] Sequestration on Various Structures of Natural Gas Hydrate Layer for Effective Recovery of $CH_4$ Gas

  • Park, Young-June;Choi, Suk-Jeong;Shin, Kyu-Chul;Seol, Ji-Woong;Lee, Hu-En
    • 한국신재생에너지학회:학술대회논문집
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    • 2006.06a
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    • pp.410-411
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    • 2006
  • On the continental margins and in permafrost regions, natural gas, which has been expected to replace petroleum energy, exists In solid hydrate farm. World hydrate reserves Including natural gas are estimated at about twice as much as the energy contained In total fossil fuel reserves. Because of its vast quantities, the efficient recovery of natural gas from natural gas hydrate becomes the most important factor on evaluating the economic feasibility in the sense of commercialization. It has been noted that carbon dioxide, one of the well-known green house gases, possibly can be stored in the ocean floor as a carbon dioxide hydrate. If the natural gas hydrate could be converted into carbon dioxide hydrate, natural gas hydrate deposits would serve as energy sources as well as carbon dioxide storage sites in the deep ocean sediments. In this study, we first attempted to examine the real swapping phenomenon occurring between guest molecules and various structures of gas hydrate through spectroscopic identification such as NMR spectroscopy.

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Dynamic Profile of the Copper Chaperone CopP from Helicobacter Pylori Depending on the Bound Metals

  • Hyun, Ja-shil;Park, Sung Jean
    • Journal of the Korean Magnetic Resonance Society
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    • v.20 no.3
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    • pp.76-81
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    • 2016
  • Copper is an elemental ion in living organisms. CopP from Helicobacter Pylori (HpCopP) is a copper(I)-binding protein and was suggested as regulator of copper metabolism in vivo. Previously, the metal binding property of HpCopP for Ag(I), Cu(I), and Cu(II) as well as the tertiary structure of HpCopP was shown. In this study, the dynamic profiles of HpCopP depending on metal binding were studied using ${^1H}-^{15}N$ steady-state NOE analysis. The heteroNOE experiment was performed for apo-CopP or metal-bound CopP. The obtained NOE values were analyzed and compared to figure out the effect of metals on the structural flexibility of HpCopP. As a result, Ag(I) and Cu(I) ions improved the rigidity of the structure while Cu(II) ion increased the flexibility of the structure, suggesting the oxidation of the CXXC motif decreases the structural stability of HpCopP.

Synthesis and Properties of Gemini Type's Diethylene Glycol Dicarboxylates (제미니형 디에틸렌글리콜 디카르복실레이트 류의 합성 및 특성)

  • Choi, Eun-Ji;Jeon, Young-Soo;Lee, Jae-Duk;Jeong, Noh-Hee
    • Journal of the Korean Applied Science and Technology
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    • v.27 no.3
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    • pp.257-265
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    • 2010
  • This study concerned about "Gemini type co-surfactant" which has very interesting properties with new components. They were synthesized by reaction of diethylene glycol monoethyl ether and dicarboxylic acid. The structure could be comfirmed with FT-IR and $^1H$-NMR. Surface active properties such as surface tension, evaluated cmc, cloud point, emulsing power were measured respectively at given conditions. Their surface tensions in the aqueous solution were decreased to 33~35 dyne/cm, which was lower than 39 dyne/cm of SDS, and their cmc values evaluated by surface tension method were $5.0{\times}10^{-1}\sim7.5{\times}10^{-1}$ mol/L. And the emulsifying power was excellent in jojoba oil. All of the synthesized Gemini surfactants possessed good water solubility and their cloud point were $48\sim58^{\circ}C$. As results, Gemini surfactants which were synthesized are expected to be applied as O/W emulsifiers.

Synthesis of Silicone Surfactant for Antifoamer (저기포성 실리콘 계면활성제의 합성)

  • Jeong, Noh-Hee;Son, Hyun-Gu
    • Journal of the Korean Applied Science and Technology
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    • v.25 no.2
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    • pp.115-122
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    • 2008
  • The hydrosilylation is an addition reaction of Si-H bond to unsaturated double bonds, which provides a convenient mechanism to synthesize poly(dimethylsiloxane-co-methylsiloxane)copolymer having siloxy units in polymer backbone. In this study, Poly(dimethylsiloxane-co-methylsiloxane) copolymer was synthesized through the polymerization reaction of cyclopentasiloxane with poly(methyl-hydrogen) siloxane. Silicone-hydrogen functional group of the poly(dimethylsiloxane-co-methylsiloxane) copolymer was substituted to the alkyl groups by hydrosilylation. And their structure was analyzed with FT-IR, H-NMR and GPC instruments, respectively. Surface tension of the synthetic compounds is increased from 22dyne/cm to 25dyne/cm according to increase additional EO moles. The cmc which was evaluated by surface tension was ranged $10^{-5}$ to $10^{-4}mol/L$ and it was decreased according to increase of dimethyl siloxyl content. HLB number of these surfactants was evaluated 9.5 to 11.5 range. These silicone surfactants is applied to self-emulsifier defoamer and personal care products as surface tension depressant, emulsifier, foam control agent.

A Study on the Synthesis of 2-Piperidylglycine (2-Piperidylglycine의 합성에 관한 연구)

  • Kyoo-hyun Chung;Kyu Jeung Wang;Hyung Gu Lee
    • Journal of the Korean Chemical Society
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    • v.36 no.4
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    • pp.598-602
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    • 1992
  • 2-Piperidylglycine will be a model compound for the synthesis of antitumor agent 593A. 2-Piperidylglycine may be synthesized by alkylation of glycine equivalent to C-2 position of piperidine ring. ${\delta}$-Valerolactam was reacted with trimethyl oxonium tetrafluoroborate to give 2-methoxy-1-piperideine. The imino ether was not condensed with ethyl phthalimidoacetate, one of glycine equivalents, but with ethyl nitroacetate to afford ethyl nitro-2-piperidylene acetate. The subsequent hydrogenation over Pt/C gave ethyl 2-piperidyl glycinate. Because the Z-configuration of the condensed product was assigned by nmr, the stereochemistry of ethyl 2-piperidyl glycinate different from that of Agent 593A.

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