• Title/Summary/Keyword: NMR Analysis

Search Result 1,407, Processing Time 0.033 seconds

The Properties of Flow and Compressive Strength of Mortar According In Replacement Ratio of Rapidly-Chilled Steel Slag Pine Aggregate (급냉 제강 슬래그 잔골재 대체율에 따른 모르타르의 유동성 및 압축강도 특성)

  • Cho Sung-Hyun;Kim Jin-Man;Kim Moon-Han;Han Ki-Suk
    • Journal of the Korea Concrete Institute
    • /
    • v.17 no.1 s.85
    • /
    • pp.77-84
    • /
    • 2005
  • The steel slag, a by-product which is produced by refining pig iron during the manufacture of steel, is mainly used as road materials after aging. It is necessary to age steel slag for long time in air because the reaction with water and free-CaO in steel slag could make the expansion of volume. This problem prevents steel slag from being used as aggregate for concrete. However, steel slag used in this study was controled by a air-jet method which rapidly cools substance melted at a high temperature. The rapidly-chilled method would prevent from generation of free-CaO in steel slag. This study dealt with the influence of the using rate of rapidly-chilled steel slag on flow, dosage of SP, W/C ratio, and strength of mortar by statistical experimental design. Also, the results of this experiment were approved by statistical analysis methods, such as analysis of variance and F-testing. As results of F-testing, this paper proved at $1\%$ level of significance that the more the using rate of rapidly-chilled steel slag increased, the more this affected the enhancement of flow, the decrease of dosage of SP and W/C ratio, and the development of compressive strength. Also, considering the fluidity and compressive strength of mortar, it is desirable to use $75\%$ of rapidly-chilled steel slag for river sand.

Structural Analysis of Natural Indigo Colorants Extracted from Polygonum tinctorium (천연인디고 색소의 구조분석)

  • Chung, In-Mo;Lee, Kwang-Gill;Sung, Gyou-Byung;Kim, Hyun-Bok;Nam, Sung-Hee;Hong, In-Pyo
    • Journal of Sericultural and Entomological Science
    • /
    • v.49 no.1
    • /
    • pp.8-13
    • /
    • 2007
  • Natural indigo colorants were prepared by extraction of Polygonum tinctorium which was harvested just in the blooming season(in the late of July). The components were analyzed by TLC and HPLC, and its structures were analyzed by FT-IR, EI-mass. The results obtained are summarized as follows; The natural indigo powder was dissolved in DMSO and developed in eluent, $CHCI_3/CH_3CN$(8.5:1.5 v/v) by means of TLC for its quality analysis. It was segregated into indirubin as a red colour and indigo as a blue colour. In case of HPLC analysis,. FT-IR spectrum of indirubin showed a peak for NH residue between 3200 and $3300cm^{-1}$. $^1H-NMR$ spectrum for indigo displayed AA'BB' spin system caused by indole structure between 6.5 and 7.7ppm of H4, 5, 6 and 7, and -NH proton for indirubin showed an singlet between 10.88 and 11.0ppm. EI-mass spectrum of indigo and indirubin both disclosed their molecular size as 262 and it implies that these two substances are isomer.

Characteristics and functional analysis of Bacillus strains from the fermented soybean products, Cheonggukjang (전통 발효 청국장으로부터 분리한 Bacillus 균주들의 특성 및 기능 분석)

  • Moon, Ji-Young;Kwon, Soon-Wo;Hong, Seung-Beom;Seok, Soon-Ja;Kim, Jeong-Seon;Kim, Soo-Jin
    • Korean Journal of Microbiology
    • /
    • v.51 no.3
    • /
    • pp.300-307
    • /
    • 2015
  • For selecting Bacillus strains producing high-quality Cheonggukjang, 8 strains were isolated from the different Cheonggukjang samples. Seven of them exhibited the highest 16S rRNA gene sequence similarity value of over 99.9% to Bacillus subtilis subsp. subtilis and one of them showed the similarity to B. licheniformis. All the strains showed positive activities for amylase, cellulase, protease and lipase, and 6 strains are positive for fibrinolytic activity. To confirm the safety of the strains isolated from the samples of Cheonggukjang which are manufactured by traditional method, strains were analyzed for the presence of seven toxin genes of Bacillus cereus and results were found negative. And 7 strains did not produce at all or merely produce both histamine and tyramine, the representative biogenic amines. Biogenic amine degradation analysis by HPLC revealed that, most of them exhibited tyramine degradation activity. For Cheonggukjang fermented by artificial inoculation of selected strains, fermentation property, sensory test, volatile basic nitrogen production and metabolic profiles by $^1H-NMR$ were tested. Seven strains were confirmed to make high-quality Cheonggukjang.

Studies on the Michael Addition Reaction between Secondary Amino Groups on the Silica Surface with Poly(ethylene glycol) Diacrylates (실리카 나노입자 표면에 결합된 2차 아미노기와 Poly(ethylene glycol) Diacrylate의 마이클 부가반응에 대한 연구)

  • Jeon, Ha Na;Ha, KiRyong
    • Polymer(Korea)
    • /
    • v.36 no.6
    • /
    • pp.822-830
    • /
    • 2012
  • We used dipodal type bis[3-(trimethoxysilyl)propyl]amine (BTMA) silane coupling agent to modify silica nanoparticles to introduce secondary amino groups on the silica surface. These N-H groups were reacted with three different molecular weights (M.W. = 258, 575, and 700) of poly(ethylene glycol) diacrylates to introduce different attached layer thicknesses on the silica surface by Michael addition reaction. After Michael addition reaction, we used several analytical techniques such as fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and solid state $^{13}C$ cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy to characterize introduced structures. We found almost complete Michael addition reaction of both two acrylate groups of PDGDA with N-H groups of BTMA modified silica to form ${\beta}$-amino acid esters. Between equimolar ratio of pure BTMA and pure PEGDA reaction, only one acrylate group of two acrylate groups of PEGDA reacted with N-H groups of pure BTMA to form ${\beta}$-amino acid ester and the other remaining acrylate group can be used to form a polymer later.

Ethylenediamine Complex for Stabilization of Omeprazole (오메프라졸의 안정화를 위한 에칠렌디아민 복합체 개발)

  • Oh, Sea-Jong;Kim, Eun-Young;Kim, Kil-Soo;Kim, Yuon-Jeung;Lee, Gye-Ju
    • Journal of Pharmaceutical Investigation
    • /
    • v.25 no.1
    • /
    • pp.9-17
    • /
    • 1995
  • To stabilize omeprazole(OMP), ethylenediamine(ED) complex of omeprazole(OMPED) was prepared by reaction between OMP and ED in methanol, and the complex formation was confirmed by the instrumental analysis, i.e., IR, DSC, EA, NMR, MS and XRD. The rates of decomposition of OMP and OMPED in aqueous solution and the shelf lives at standard temperature were measured by accelerated stability analysis. The results are summarized as follows; The mole ratio of OMP and ED in OMPED complex is 1:1, the energy of formation within OMPED might be combined between polar imidazole group of OMP with induced a dipole amine group in the readily polarizable ED molecule. At standard temperature the degradation rate constant of OMP in aqueous solution is $2.540{\times}10^{-2}\;hr^{-1}$ and the shelf life is 4.15 hrs, and in the case of OMPED the degradation rate constant is $7.986{\times}10^{-4}\;hr^{-1}$ and the shelf life is 131.96 hrs. So, the OMPED has about 31 times longer shelf life than OMP. The activation energy of OMP and OMPED are 5.23 and 18.55 kcal $mole^{-1}$ respectively. The stability of OMP is dependent chiefly on pH in the solutions and it decomposes readily in acidic medium by hydrogen ion catalized reaction but becomes stable beyond pH 9.0. In case of the ED-complex, OMPED is stable in neutral as well as in dilute acidic solutions even in pH 6, OMPED is very stable to light(UV), that is, the rate constant and shelf life of OMP are $k=1.0188{\times}10^{-2}\;day^{-1}$, $T_{90%}=4.5 \;days$, on the other hand, the those of OMPED are $k=7.138{\times}10^{-4}\;day^{-1}$, $T_{90%}=64.1\;days$, respectively. From the above results, it is thought that new dosage forms could be developed by using the OMPED as a potential OMP complex.

  • PDF

Formation of New Thorium (IV) Complexes with Crown Ethers (새로운 Thorium (IV)-Crown Ether 착물형성)

  • Jung, Hak-Jin;Jung, Oh-Jin;Suh, Hyouck-Choon
    • Journal of the Korean Chemical Society
    • /
    • v.31 no.3
    • /
    • pp.258-270
    • /
    • 1987
  • A series of new thorium nitrate complexes with crown ethers have been synthesized from the reaction of the hydrated thorium nitrate, with the appropriate crown ethers of different cavity sizes in various solvents such as methanol, ethanol, butanol, methylacetate, acetone, tetrahydrofuran and acetylacetone. CHN elemental analysis, ICPAS, thermal analysis and Karl-Fischer method have been used to characterize their compositions, and the spectroscopic methods of IR, UV, $^1H-NMR$, and X-ray diffraction have been employed to determine the structures and solvolysis phenomena of these complexes. and the electrical conductances were measured in DMSO, and water solvent. The solvolysis have been observed only in the complexes synthesized in acetylacetone solvent. In the solvated complexes of 15-crown-5 and 18-crown-6, the mole ratio of $Th^{4+}$: ligand : acetylacetone is found to be 1:1:1, but in the non-solvated complexes of 12-crown-4 and 15-crown-5, the mole ratios of Th:L are 1:2 and 2:3, respectively, and that in the complexes of both 18-crown-6 and dicyclohexano-18-crown-6 is 1:1. All complexes which were not solvated have shown $n{\to}{\sigma}^{\ast}$ electronic transitions of crown ether whereas complexes solvated have exhibited both $n{\to}{\sigma}^{\ast}$ of crown ether and $n{\to}{\pi}^{\ast}$ transitions of acac. The dissociation mole ratio of $Th^{4+}$ and nitrate ion is found to be 1:1 in aprotic solvent, and 1:4 in protic solvent like water.

  • PDF

Molecular Mechanism of Crocin Induced Caspase Mediated MCF-7 Cell Death: In Vivo Toxicity Profiling and Ex Vivo Macrophage Activation

  • Bakshi, Hamid A;Hakkim, Faruck Lukmanul;Sam, Smitha
    • Asian Pacific Journal of Cancer Prevention
    • /
    • v.17 no.3
    • /
    • pp.1499-1506
    • /
    • 2016
  • Background: Crocus sativus and its major constituent crocin are well established to have anti-cancer properties in breast cancer cells (MCF-7). However the role of C. sativus extract (CSE) and crocin on caspase signaling mediated MCF-7 cell death at molecular level is remains unclear. In this study, we tried to unravel role of CSE and crocin on caspase mediated MCF-7 cells death and their in vivo preclinical toxicity profiling and immune stimulatory effect. Materials and Methods: CSE extract was fractionated by HPLC and crocin was isolated and characterized by NMR, IR, and MS. MCF-7 cells were treated with both CSE and crocin and expression of Bcl-2 and Bax was assessed after 24 and 36 hours. Furthermore, caspase 3, caspase 8 and caspase 9 expression was determined by Western blotting after 24 hours of treatment. DNA fragmentation analysis was performed for genotoxicity of CSE and crocin in MCF-7 cells. The in vivo toxicity profile of CSE (300 mg/kg of b.wt) was investigated in normal Swiss albino mice. In addition, peritoneal macrophages were collected from crocin (1, 1.5 and 2 mg/kg body weight) treated mice and analyzed for ex vivo yeast phagocytosis. Results: Immunoblot analysis revealed that there was time dependent decline in anti-apoptotic Bcl-2 with simultaneous upregulation of Bax in CSE and crocin treated MCF-7 cells. Further CSE and crocin treatment downregulated caspase 8 and 9 and cleaved the caspase 3 after 24 hours. Both CSE and crocin elicited considerable DNA damage in MCF-7 cells at each concentration tested. In vivo toxicity profile by histological studies revealed no observable histopathologic differences in the liver, kidney, spleen, lungs and heart in CSE treated and untreated groups. Crocin treatment elicited significant dose and time dependent ex vivo yeast phagocytosis by peritoneal macrophages. Conclusions: Our study delineated involvement of pro-apoptotic and caspase mediated MCF-7 cell death by CSE and crocin at the molecular level accompanied with extensive DNA damage. Further we found that normal swiss albino mice can tolerate the maximum dose of CSE. Crocin enhanced ex vivo macrophage yeast phagocytic ability.

Complex Formation of Transition and Post-Transition Metal Ions with 1,15-Diaza-3,4 : 12,13-dibenzo-5,8,11-trioxacyclooctadecane (전이 및 중금속이온과 1,15-diaza-3,4 : 12,13-dibenzo-5,8,11-trioxa-cyclooctadecane과의 착물형성)

  • Kim, Si-Joong;Lee, Myung-Jae;Koo, Chang-Hyung;Woo, Kyoun-Ja
    • Journal of the Korean Chemical Society
    • /
    • v.35 no.6
    • /
    • pp.645-652
    • /
    • 1991
  • The stability constants$(K_f)$ of the complexes of some transition and post-transition metal ions (Co(Ⅱ), Ni(Ⅱ), Cu(Ⅱ), Zn(Ⅱ), Cd(Ⅱ), Pb(Ⅱ), Hg(Ⅱ)) with $N_2O_3$-donor macrocyclic ligand, 1,15-diaza-3,4 : 12,13-dibenzo-5,8,11-trioxacyclooctadecane ($NtnOdienH_4$), have been determined by potentiometry in aqueous solution at $25^{\circ}C$. Log $K_f$ values of the complexes were : Co(Ⅱ): 3.83, Ni(Ⅱ) : 4.56, Cu(Ⅱ) : 7.74, Zn(Ⅱ) : 4.98, Cd(Ⅱ) : 3.91, Pb(Ⅱ) : 6.65, and Hg(Ⅱ) : 14.87. The order of stabilities of transition metal complexes was the same as the natural order of stability proposed by Williams-Irving. In post-transition metal complexes, the order of stabilities was Cd(Ⅱ) < Pb(Ⅱ) < Hg(Ⅱ), and the covalent character in metal ion-donor atoms bonds appeared a dominant factor in the stability. In methanol solution, each metal ion forms 1 : 1 complex, while Ni(Ⅱ) ion forms both 1 : 1 and 1 : 2 complexes. It was confirmed by $^1H-$ and $^{13}C-$NMR spectral study that the nitrogen atoms in the ligand were major contributors for the complexation of post-transition metal ions with the ligand. It was shown, by elementry analysis, electrical conductivity and magnetic susceptibility measurements, and spectral analysis, that solid Cu(Ⅱ)-and Zn(Ⅱ)-complexes have a distorted octahedral and a tetrahedral structure, respectively.

  • PDF

New Ruthenium Complexes for Semiconductor Device Using Atomic Layer Deposition

  • Jung, Eun Ae;Han, Jeong Hwan;Park, Bo Keun;Jeon, Dong Ju;Kim, Chang Gyoun;Chung, Taek-Mo
    • Proceedings of the Korean Vacuum Society Conference
    • /
    • 2014.02a
    • /
    • pp.363-363
    • /
    • 2014
  • Ruthenium (Ru) has attractive material properties due to its promising characteristics such as a low resistivity ($7.1{\mu}{\Omega}{\cdot}cm$ in the bulk), a high work function of 4.7 eV, and feasibility for the dry etch process. These properties make Ru films appropriate for various applications in the state-of-art semiconductor device technologies. Thus, it has been widely investigated as an electrode for capacitor in the dynamic random access memory (DRAM), a metal gate for metal-oxide semiconductor field effect transistor (MOSFET), and a seed layer for Cu metallization. Due to the continuous shrinkage of microelectronic devices, better deposition processes for Ru thin films are critically required with excellent step coverages in high aspect ratio (AR) structures. In these respects, atomic layer deposition (ALD) is a viable solution for preparing Ru thin films because it enables atomic-scale control of the film thickness with excellent conformality. A recent investigation reported that the nucleation of ALD-Ru film was enhanced considerably by using a zero-valent metallorganic precursor, compared to the utilization of precursors with higher metal valences. In this study, we will present our research results on the synthesis and characterization of novel ruthenium complexes. The ruthenium compounds were easy synthesized by the reaction of ruthenium halide with appropriate organic ligands in protic solvent, and characterized by NMR, elemental analysis and thermogravimetric analysis. The molecular structures of the complexes were studied by single crystal diffraction. ALD of Ru film was demonstrated using the new Ru metallorganic precursor and O2 as the Ru source and reactant, respectively, at the deposition temperatures of $300-350^{\circ}C$. Self-limited reaction behavior was observed as increasing Ru precursor and O2 pulse time, suggesting that newly developed Ru precursor is applicable for ALD process. Detailed discussions on the chemical and structural properties of Ru thin films as well as its growth behavior using new Ru precursor will be also presented.

  • PDF

Isolation of Anticarcinogenic Isoflavone-conjugated Glycoproteins from a Submerged Liquid Culture of Agaricus blazei Mycelia by the Autolysis Process (신령버섯균사체 액체배양물의 자가분해에 의한 항암성 isoflavone-conjugated glycoprotein 분리)

  • Kim, So Young;Kim, Young Suk;Jang, Joung Soon;Kim, Boh Hyun;Rakib, Abdur Md.;Kim, Gon Sup;Kim, Jeong Ok;Ha, Yeong Lae
    • Journal of Life Science
    • /
    • v.24 no.12
    • /
    • pp.1316-1324
    • /
    • 2014
  • Most beta-glucans obtained from various fruit bodies of mushrooms and mushroom mycelial cultures have high-molecular weight glycoproteins, conjugated with beta-glucans. We report that isoflavone-conjugated glycolproteins (designated as gluvone) were isolated and exhibited stronger anticarcinogenic activities. Agaricus blazei mycelia (ABM) was cultured in a liquid medium containing soybean flakes for 14 days. The liquid culture was autolyzed by incubating at $53^{\circ}C$ (pH 5.5) for 3 h. A crude glycoprotein (CGP) fraction with a cytotoxic effect on a mouse ascite cancer cell line (S-180) and a human breast cancer cell line (MCF-7) was isolated from the autolyzed ABM cultures by 80% ethanol treatment. Gluvone was isolated from the CGP with Sephadex G-75 column chromatography. It exhibited a stronger anticancer effect than CGP against the S-180 cell-induced female ICR mouse ascites carcinogenesis. Gluvone with 9,400 daltons was identified as a glycoprotein conjugated with isoflavone. According to HPLC and GC analysis, in conjunction with $^1H$-NMR spectral analysis, it contained 60% carbohydrates (glucose, fructose, and ribose), 31% protein, and 2% isoflavone (daidzein and genistein), which is a novel material. These results indicate that a strong anticarcinogenic gluvone was isolated from the autolyzed product of a submerged liquid culture of ABM, suggesting that autolysis could be a useful tool to produce antitumor agents.