• 제목/요약/키워드: NMR measurements

검색결과 157건 처리시간 0.028초

광물성 한약으로 이용되는 양기석, 연옥,음기석의 분광학적 및 자기적 특성 (Spectmscopic and Magnetic Properties of Yanggiseok, Yeonok and Eumgiseok used as Mineral Medicine)

  • 김선옥;박맹언;정율필
    • 자원환경지질
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    • 제35권4호
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    • pp.317-323
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    • 2002
  • 양기와 음기를 보하는 약재로 알려진 양기석과 음기석 및 연옥에 대한 의료적 활용을 파악하고, 광물학적 특성, 분광학적 및 자기적 특성을 규명하기 위하여 X선 형광분석, X-선 회절분석, 주사전자현미경, 적외선 분광분석, 핵자기 공명분석 및 감응자기력을 실시하였다. 광물성 한약으로 사용되는 양기석은 양기석으로 확인되었으뗘, 연옥은 투각섬석으로 구성되었다. 또한, 음기석은 주로 질석으로 구성되며, 소량의 카올리나이트와 할로이사이트를 함유하였다. 사슬형 규산염 중 각섬석군에 속하는 이들 연옥과 양기석은 유사한 범위의 분광학적 특성을 가지며, 연옥은 4$0^{\circ}C$에서 방사에너지가 큰 반면, 양기석은 15$0^{\circ}C$에서 방사에너지가 크다 음기석은 각섬석군의 광물보다 4$0^{\circ}C$와 15$0^{\circ}C$에서 모두 낮은 방사에너지를 나타내었다. 광물성 한약을 증류수에 20일간 침적한 후에 측정한 NMR분석에서의 선폭은 음기석, 양기석, 연옥의 순으로 감소되나, 80일이 경과한 후의 결과는 음기석, 연옥, 양기석 순으로 감소하였다. 양기석과 음기석은 가열 온도가 높아짐에 따라 감응 자기력 값이 대체적으로 증가하고, 연옥은 감소하는 경향을 나타내었다. 광물별로는 상온과 가열시 모두 음기석, 양기석, 연옥의 순으로 감소하였다.

광역학적/광열치료 응용을 위한 광증감제가 결합한 골드 나노로드의 합성 및 특성분석 (Synthesis and Characterization of Photosensitizer-conjugated Gold Nanorods for Photodynamic/Photothermal Therapy)

  • 최종선;김소연
    • 공업화학
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    • 제27권6호
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    • pp.599-605
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    • 2016
  • 최근 효과적인 암 치료 방법으로 광역학치료(photodynamic therapy)와 광열치료(photothermal therapy)가 주목받고 있다. 본 연구에서는 광열치료에 필요한 광열인자로써의 역할을 할 수 있는 골드 나노로드(AuNR)를 합성하고, 그 표면에 광역학치료를 위한 광증감제(photosensitizer)를 결합하였다. 즉, 골드 나노로드를 체내에 오래 머무르도록 하기 위해 PEG(polyethylene glycol) 및 효과적인 암 표적지향성을 위해 FA (folic acid) 리간드를 도입하였고, FA-PEG와 poly-${\beta}$-benzyl-L-aspartate (PBLA)로 이루어진 블록 공중합체를 3,4-dihydroxy hydrocinnamic acid (HCA) linker를 사용하여 골드 나노로드의 표면개질을 하였다. 또한 $AgNO_3$의 feeding ratio 변화를 통해 다양한 aspect ratio를 갖는 골드 나노로드를 합성하였고, UV-visible spectrophotometer, $^1H$-NMR, XPS, TEM 분석을 통해 FA-PEG-$P(Asp)_{50}$-HCA-AuNR100의 물리 화학적 특성과 morphology를 분석하였고, 성공적인 표면 개질을 확인할 수 있었다. 골드 나노로드의 표면 개질을 통한 생체 적합성 약물전달체의 합성은 효과적인 암 진단 및 다양한 광역학/광열치료 분야에 응용이 될 수 있을 것으로 기대된다.

Study of the Molecular Reorientation in Ammonium Sulfate by Neutron Scattering

  • Kim, Huhn-Jun
    • Nuclear Engineering and Technology
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    • 제4권4호
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    • pp.306-321
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    • 1972
  • 중성자산란을 이용하여 (NH$_4$)$_2$SO$_4$에 있어서 분자의 재배향(reorientation)을 조사하였다. T=300$^{\circ}$K의 측정에 대해서는 여러산란각도에서 분리된 준탄성산란스펙트럼과 구조인자(form-factor)를 SKOLD 이론에 의한 네개의 재배향모형과 비교하여 NH$_4$이온이 $\tau$$_{c}$=2.0$\times$$10^{-11}$ sec인 3중회전 4축(3-fold four axes) 또는 2중회전 3축재배향을 한다는 결론을 얻었다. $\tau$$_{c}$의 온도의존성을 100$^{\circ}$K-413$^{\circ}$K에 걸쳐 조사했으며, 고온상에 대해서는 복합스책트럼의 폭을 NMR이완시간측정에 얻은 결론과 비교하였다. 이상의 결과는 중성자산란이 고체에 있어서 분자재배향의 상세한 조사에 유력한 한 방법임을 보여 주었으며 따라서 이 방법의 응용에 대한 고찰을 하였다. 그 한 예로서 NH$_4$I(상 1)에 대해서 측정한 탄성구조인자와 자유회전근사에서 얻은 이론치를 비교하여 NH$_4$이온이 8면체형포텐샬 (Potential)에서 $\tau$$_{c}$$\leq$$10^{-12}$ sec인 재배향을 하고 있음을 주장하였다. 분자재배향이 비탄성 스펙트럼에 미치는 영향에 대하여 간단한 이론적 고찰을 하였다.을 하였다.

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Synthesis and Spectroscopic Characterization of Manganese(II), Iron(III) and Cobalt(III) Complexes of Macrocyclic Ligand. Potential of Cobalt(III) Complex in Biological Activity

  • El-Tabl, Abdou S.;Shakdofa, Mohamad M.E.;El-Seidy, Ahmed M.A.
    • 대한화학회지
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    • 제55권6호
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    • pp.919-925
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    • 2011
  • A new series of manganese(II), iron(III) and cobalt(III) complexes of 14-membered macrocyclic ligand, (3,6,10,13,16,19-hexaazabicyclo[6.6.6]icosane-1,8-diamine) have been prepared and characterized by elemental analyses, IR, UV-VIS, $^1H$- and $^{13}C$- NMR spectra, magnetic susceptibilities, conductivities, and ESR measurements. Molar conductance measurements in DMF solution indicate that the complexes are electrolytes. The ESR spectrum for cobalt(III) complex in $CD_3OD+10%D_2O$ after exposure to $^{60}Co-{\gamma}$-rays at 77 K using a 0.2217 M rad $h^{-1}$ vicrad source showed $g_{\perp}$ > $g_{\parallel}$ > $g_e$, indicating that, the unpaired electron site is mainly present in the $d_z2$ orbital with covalent bond character. In this case, the ligand hyperfine tensors are nearly collinear with ${\gamma}$-tensors, so there is no major tendency to bend. Therefore, little extra delocalization via the ring lobe of the $dz^2$ orbital occurs. However, the ESR spectrum in solid state after exposure to $^{60}Co-{\gamma}$-rays at 77 K showed $g_{\parallel}$ > $g_{\perp}$ > $g_e$, indicating that, the unpaired electron site is mainly present in the $d_x2_{-y}2$ ground state as the resulting spectrum contains a large number of randomly oriented molecules provided that, the principle directions of g and A tensors. Manganese (II) complex 2, $[H_{12}LMn]Cl_4.2H_2O$, showed six isotropic lines characteristic to an unpaired electron interacting with a nucleus of spin 5/2, however, iron(III) complex 3, $[H_{12}LFe]Cl_5.H_2O$, showed spectrum of a high spin $^{57}Fe$ (I=1/2), $d^5$ configuration. The geometry of these complexes was supported by elemental analyses, IR, electronic and ESR spectral studies. Complex 1 showed exploitation in reducing the amount of electron adducts formed in DNA during irradiation with low radiation products.

Synthetic, Characterization, Biological, Electrical and Catalytic Studies of Some Transition Metal Complexes of Unsymmetrical Quadridentate Schiff Base Ligand

  • Maldhure, A. K.;Pethe, G. B.;Yaul, A. R.;Aswar, A. S.
    • 대한화학회지
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    • 제59권3호
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    • pp.215-224
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    • 2015
  • Unsymmetrical tetradentate Schiff base N-(2-hydroxy-5-methylacetophenone)-N'-(2-hydroxy acetophenone) ethylene diamine (H2L) and its complexes with Cr(III), Mn(II), Fe(III), Co(II), Ni(II) and Cu(II) have been synthesized and characterized by elemental analyses, magnetic susceptibility measurements, IR, electronic spectra and thermogravimetric analyses. 1H, 13C-NMR and FAB Mass spectra of ligand clearly indicate the presence of OH and azomethine groups. Elemental analyses of the complexes indicate that the metal to ligand ratio is 1:1 in all complexes. Infrared spectra of complexes indicate a dibasic quadridentate nature of the ligand and its coordination to metal ions through phenolic oxygen and azomethine nitrogen atoms. The thermal behavior of these complexes showed the loss of lattice water in the first step followed by decomposition of the ligand in subsequent steps. The thermal data have also been analyzed for the kinetic parameters by using Horowitz-Metzger method. The dependence of the electrical conductivity on the temperature has been studied over the temperature range 313-403 K and the complexes are found to show semiconducting behavior. XRD and SEM images of some representative complexes have been recorded. The antimicrobial activity of the ligand and its complexes has been screened against various microorganisms and all of them were found to be active against the test organisms. The Fe(III) and Ni(II) complex have been tested for the catalytic oxidation of styrene.

Synthesis and Characterization of Biodegradable Elastic Hydrogels Based on Poly(ethylene glycol) and Poly(${\varepsilon}-caprolactone$) Blocks

  • Im, Su-Jin;Choi, You-Mee;Subramanyam, Elango;Huh, Kang-Moo;Park, Ki-Nam
    • Macromolecular Research
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    • 제15권4호
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    • pp.363-369
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    • 2007
  • Novel biodegradable elastic hydrogels, based on hydrophilic and hydrophobic polymer blocks, were synthesized via the radical crosslinking reaction of diacrylates of poly(ethylene glycol) (PEG) and poly(${\varepsilon}-caprolactone$) (PCL). PEG and PCL diols were diacrylated with acryloyl chloride in the presence of triethylamine, with the reaction confirmed by FT-IR and $^1H-NMR$ measurements. The diacrylate polymers were used as building-blocks for the syntheses of a series of hydro gels, with different block compositions, by simply varying the feed ratios and molecular weights of the block components. The swelling ratio of the hydrogels was controlled by the balance between the hydrophilic and hydrophobic polymer blocks. Usually, the swelling ratio increases with increasing PEG content and decreasing block length within the network structure. The hydrogels exhibited negative thermo-sensitive swelling behavior due to the coexistence of hydrophilic and hydrophobic polymer components in their network structure, and such thermo-responsive swelling/deswelling behavior could be repeated using a temperature cycle, without any significant change in the swelling ratio. In vitro degradation tests showed that degradation occurred over a 3 to 8 month period. Due to their biodegradability, biocompatibility, elasticity and functionality, these hydrogels could be utilized in various biomedical applications, such as tissue engineering and drug delivery systems.

Synthesis, Characterization and DNA Interaction Studies of (N,N'-Bis(5-phenylazosalicylaldehyde)-ethylenediamine) Cobalt(II) Complex

  • Sohrabi, Nasrin;Rasouli, Nahid;Kamkar, Mehdi
    • Bulletin of the Korean Chemical Society
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    • 제35권8호
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    • pp.2523-2528
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    • 2014
  • In the present study, at first, azo Schiff base ligand of (N,N'-bis(5-phenylazosalicylaldehyde)-ethylenediamine) ($H_2L$) has been synthesized by condensation reaction of 5-phenylazosalicylaldehyde and ethylenediamine in 2:1 molar ratio, respectively. Then, its cobalt complex (CoL) was synthesized by reaction of $Co(OAc)_2{\cdot}4H_2O$ with ligand ($H_2L$) in 1:1 molar ratio in ethanol solvent. This ligand and its cobalt complex containing azo functional groups were characterized using elemental analysis, $^1H$-NMR, UV-vis and IR spectroscopies. Subsequently, the interaction between native calf thymus deoxyribonucleic acid (ct-DNA) and CoL complex was investigated in 10 mM Tris/HCl buffer solution, pH = 7 using UV-vis absorption, thermal denaturation technique and viscosity measurements. From spectrophotometric titration experiments, the binding constant of CoL complex with ct-DNA was found to be $(2.4{\pm}0.2){\times}10^4M^{-1}$. The thermodynamic parameters were calculated by van't Hoff equation.The enthalpy and entropy changes were $5753.94{\pm}172.66kcal/mol$ and $43.93{\pm}1.18cal/mol{\cdot}K$ at $25^{\circ}C$, respectively. Thermal denaturation experiments represent the increasing of melting temperature of ct-DNA (about $0.93^{\circ}C$) due to binding of CoL complex. The results indicate that the process is entropy-driven and suggest that hydrophobic interactions are the main driving force for the complex formation.

Neuraminidase Inhibitors from the Fruiting Body of Phellinus igniarius

  • Kim, Ji-Yul;Kim, Dae-Won;Hwang, Byung Soon;Woo, E-Eum;Lee, Yoon-Ju;Jeong, Kyeong-Woon;Lee, In-Kyoung;Yun, Bong-Sik
    • Mycobiology
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    • 제44권2호
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    • pp.117-120
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    • 2016
  • During our ongoing investigation of neuraminidase inhibitors from medicinal fungi, we found that the fruiting bodies of Phellinus igniarius exhibited significant inhibitory activity against neuraminidase from recombinant H3N2 influenza viruses. Two active compounds were isolated from the methanolic extract of P. igniarius through solvent partitioning and Sephadex LH-20 column chromatography. The active compounds were identified as phelligridins E and G on proton nuclear magnetic resonance ($^1H$ NMR) and electrospray ionization mass measurements. These compounds inhibited neuraminidases from recombinant rvH1N1, H3N2, and H5N1 influenza viruses, with $IC_{50}$ values in the range of $0.7{\sim}8.1{\mu}M$.

전기적 활성을 갖는 폴리티오펜 유도체들의 합성과 생체계면에의 응용 (I) (Synthesis of Electroactive Polythiophene Derivatives and Its Application for Biointerface (I))

  • 정선형;배진영;김지흥;정동준
    • 폴리머
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    • 제26권1호
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    • pp.28-36
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    • 2002
  • 본 연구에서는 바이오칩 등에 응용 가능한 전도성 고분자 필름을 제조하기 위해 3-triophene acetic acid을 선택하여, 쉽게 전기적으로 산화되어 전기적 활성을 나타내는 고분자들을 형성하였다. 3-Thiophene acetic acid에 있는 카르복실기의 보호기들은 solid state에서 쉽게 제거되어질 수 있고, 그 결과 반응성 카르복실기가 전기적 활성을 나타내는 고분자 표면 위에 재생되어질 수 있었다. 즉, 카르복실기의 보호를 통한 전기중합과 뒤이은 보호기의 제거로 반응성인 카르복실기를 갖는 새로운 고분자 담체를 제조할 수 있었고, 기존의 방법으로 합성한 macromonomer를 필름 표면에 도입하여 전기적 활성을 나타내며 동시에 고분자 전해질이 도입된 전도성 고분자 필름을 얻었다. 합성한 전도성 단량체들과 macromonomer의 도입여부는 FT-IR과 $^1H-NMR$ 및 ESCA측정으로 확인하였고, 전극표면에 형성된 필름들의 형태는 SEM을 통해서 관찰하였다. 전기적 활성은 cyclic voltammogram(CV)을 통하여 확인하였으며, 얻어진 고분자 필름들은 0.7~0.9 V의 영역에서 전형적인 poly(3-alkylthiophene)의 전기 화학적 거동을 나타내었다.

Ergosterol Peroxide from Flowers of Erigeron annuus L.as an Anti-Atherosclerosis Agent

  • Kim, Dong-Hyun;Jung, Sung-Je;Chung, In-Sik;Lee, Youn-Hyung;Kim, Dae-Keun;Kim, Sung-Hoon;Kwon, Byoung-Mog;Jeong, Tae-Sook;Park, Mi-Hyun;Seoung, Nak-Sul;Baek, Nam-In
    • Archives of Pharmacal Research
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    • 제28권5호
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    • pp.541-545
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    • 2005
  • Flowers of Erigeron annuus L. were extracted with 80% aqueous MeOH, and the concentrated extract was partitioned with EtOAc, n-BuOH, and H$_2$O. Repeated silica gel and OD S column chromatography of the EtOAc fraction led to the isolation of a sterol, through activityguided fractionation, using ACAT inhibitory activity measurements. From the physico-chemical data, including NMR, MS, and IR, the chemical structure of the compound was determined to be an ergosterol peroxide (1), which has been isolated for the first time from this plant. This compound exhibited hACAT-1 and Lp-PLA$_2$ inhibitory effects, with inhibitory values of 51.6 ${\pm}$ 0.9 and 51 .7 ${\pm}$ 1.2%, at a treatment concentration of 0.23 mM.