• Title/Summary/Keyword: NMR measurements

Search Result 157, Processing Time 0.025 seconds

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

  • 김선옥;박맹언;정율필
    • Economic and Environmental Geology
    • /
    • v.35 no.4
    • /
    • pp.317-323
    • /
    • 2002
  • Mineral medicines are single or mixtures of minerals and rocks which have been used to treat disease. Recently, their application has been increased by emphasizing the physical properies of the medicines, in addition to their chemical properies. In this study, mineralogical, chemical, spectroscopic and magnetic properties were measured using X-ray diffraction analysis, X-ray fluorescence spectrometry, Ff-Infrared spectroscopy, nuclear magnetic resonance spectroscopy, mass magnetic susceptibility. Experiments were done using these properties to evaluate application of traditional mineral medicines such as Yanggiseok, Yeonok and Eumgiseok. Mineralogical study proves that Yanggiseok, generally known as tremolite, consists of actinolite. Yeonok for medical usage mostly consists of fine grained tremolite. Eumgiseok is mainly composed of vermiculite and minor kaolinite and halloysite. Yeonok and Yanggiseok, belong to the amphibole group among inosilicates and both have similar emission power properties. The intensity of emission power, calculated from FT-IR measurements, follows in the order of Yeonok, Yanggiseok and Eumgiseok at 40$^{\circ}$C and Yanggiseok, Yeonok and Eumgiseok in such order at 150$^{\circ}$C. As a result of NMR analysis after 20 days in distilled water, the three mineral medicines decreased in the following order; Eumgiseok, Yanggiseok and Yeonok. However, the same minerals decreased in the order of Eumgiseok, Yeonok and Yanggiseok after 80 days. In response temperature, magnetic susceptibility of Yanggiseok and Eumgiseok systematically increased by heating to 25$^{\circ}$C, 100$^{\circ}$C and 700$^{\circ}$C. Magnetic susceptibility of Yeonok shows a decreasing pattern due to heating.

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

  • Choi, Jongseon;Kim, So Yeon
    • Applied Chemistry for Engineering
    • /
    • v.27 no.6
    • /
    • pp.599-605
    • /
    • 2016
  • Recently, photodynamic and photothermal therapies have received increasing attention as an effective cancer treatment. In this study, a gold nanorod (AuNR) colloidal solution was synthesized as a hyperthermia agent for photothermal therapy and also modified with photosensitizer (PS) for photodynamic therapy. PEG (polyethylene glycol) and FA (folic acid) ligand were also introduced into AuNR for the long circulation in human body and efficient targeting of cancer cells, respectively and AuNRs were modified with FA-PEG and poly-${\beta}$-benzyl-L-aspartate (PBLA) block copolymers through a 3,4-dihydroxy hydrocinnamic acid (HCA) linker. A series of AuNRs with various aspect ratios were synthesized by controlling the feeding ratio of $AgNO_3$. The physicochemical property and morphology of synthesized AuNR100 and FA-PEG-$P(Asp)_{50}$-HCA-AuNR100 were analyzed by UV-visible spectrophotometer, $^1H$ NMR, XPS measurements, TEM. The surface modified AuNR carrier with biocompatibility could be applied for the effective diagnosis as well tumor phototherapy.

Study of the Molecular Reorientation in Ammonium Sulfate by Neutron Scattering

  • Kim, Huhn-Jun
    • Nuclear Engineering and Technology
    • /
    • v.4 no.4
    • /
    • pp.306-321
    • /
    • 1972
  • Molecular reorientation in (NH$_4$)$_2$SO$_4$, has been studied by cold neutron scattering. For T=300$^{\circ}$K data, the isolated quasielastic spectra and form-factors at various scattering angles are compared with four reorientational models based on SKOLD theory. Front these, it is concluded that the NH$_4$ions are performing either 3-fold four axes or 2-fold three axes reorientation with $\tau$$_{c}$=2.0$\times$10$^{-11}$ sec. The temperature dependence of f. is studied over 100$^{\circ}$K-413$^{\circ}$K and for the high-temperature phase, the widths of composite spectra are compared with the results from NMR relaxation measurements. All the results have shown that the neutron scattering method is capable of giving detalis of the reorientational modes in solids and therefore some discussions are given on the application of this method. A study of the form-factor is applied for NH$_4$I (Phase I) by comparing the measurement with the calculation based on free rotation approximation and proposed a reorientation model of NH$_4$ ions in the octahedral potential cage with $\tau$$_{c}$$\leq$10$^{-12}$ sec. Also a brief theoretical prediction for the effect of reorientational motions on the inelastic spectrum is discussed.sed.

  • PDF

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.
    • Journal of the Korean Chemical Society
    • /
    • v.55 no.6
    • /
    • pp.919-925
    • /
    • 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.
    • Journal of the Korean Chemical Society
    • /
    • v.59 no.3
    • /
    • pp.215-224
    • /
    • 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
    • /
    • v.15 no.4
    • /
    • pp.363-369
    • /
    • 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
    • /
    • v.35 no.8
    • /
    • pp.2523-2528
    • /
    • 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
    • /
    • v.44 no.2
    • /
    • pp.117-120
    • /
    • 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 $0.7{\sim}8.1{\mu}M$.

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

  • 정선형;배진영;김지흥;정동준
    • Polymer(Korea)
    • /
    • v.26 no.1
    • /
    • pp.28-36
    • /
    • 2002
  • In this study, we synthesized novel thiophene derivatives by the protection of the carboxyl group of 3-thiophene acetic acid with differently substituted benzyl groups. While 3-thiophene acetic acid is not electro-polymerizable, the modified monomers can be easily electro-oxidized to form stable electroactive polymers. The protecting groups can be easily removed in the solid state and the desired reactive carboxyl group can be introduced on the polymer surface. SEM observations show that obtained polymer films show a very good film surface and homogeneous morphology on the Pt electrode. After introduction of macromonomer, FT-IR spectrum shows new absorption bands at 1650 and $1550 cm^{-1}$, which is consistent with the formation of an amide bond. Electroactivity measurements were examined by cyclic voltammogram(CV). These polymers showed the characteristic electrochemical behavior of poly(3-alkylthiophene)s with reversible redox transition in the range of 0.7-0.9 V.

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
    • /
    • v.28 no.5
    • /
    • pp.541-545
    • /
    • 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.