• Title/Summary/Keyword: techniques%3A spectroscopic

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Spectroscopic Comparison of Photo-oxidation of Outside and Inside of Hair by UVB Irradiation (자외선B 조사에 의한 모발 외부와 내부의 광산화에 관한 분광학적 비교)

  • Ha, Byung-Jo
    • Applied Chemistry for Engineering
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    • v.31 no.2
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    • pp.220-225
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    • 2020
  • Hair is made of proteins containing various amino acids. Ultraviolet (UV) radiation is believed to be responsible for the most damaging effects of sunlight, and also plays an important role in hair aging. The purpose of this study was to investigate the changes in morphological and chemical structures after ultraviolet B (UVB) irradiation of human hair. The UVB-irradiated hair showed characteristic morphological and structural changes, compared to those of the normal hair. The result from a scanning electron microscope (SEM) equipped with an energy dispersive X-ray diffractometer (EDX) showed that the scale of UV-irradiated hair appeared to be rough and the amount of oxygen element was higher than that of the normal hair. Fluorescence and three dimensional (3D) topographical images were obtained by a confocal laser scanning microscope (CLSM). In 3D images, the green emission intensity of normal hair was much higher than that of fluorescing UVB-irradiated hair. The intensity of green emission reflects the intrinsic fluorescence of hair protein. Also, a fluorescent imaging method using fluorescamine reagent was used to identify the free amino groups resulting from a peptide bond breakage in UVB-irradiated hair. Strong blue fluorescence of UVB-irradiated hair, which indicates a very high level of amino groups, was observed by CLSM. Therefore, the fluorescamine as an extrinsic fluorescence could provide a useful tool to identify the peptide bond breakage in UVB-irradiated hair. Infrared image mapping was also employed to assess the cross-sections of normal and UVB-irradiated specimens to examine the oxidation of disulfide bonds. The degree of peak areas with strong absorbance for the disulfide mono-oxide was spread from the outside to the inside of hair. The spectroscopic techniques used alone, or in combination, launch new possibilities in the field of hair cosmetics.

Synthesis of CoTiOx and Its Catalytic Activity in Continuous Wet TCE Oxidation (CoTiOx의 합성 및 연속 습식 TCE 산화반응에서의 촉매활성)

  • Kim, Moon-Hyeon
    • Journal of Environmental Science International
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    • v.16 no.12
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    • pp.1431-1437
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    • 2007
  • Cobalt titanates($CoTiO_x$), such as $CoTiO_3$ and $Co_2TiO_4$, have been synthesized via a solid-state reaction and characterized using X-ray diffraction(XRD) and X-ray photoelectron spectroscopic(XPS) measurement techniques, prior to being used for continuous wet trichloroethylene(TCE) oxidation at $36^{\circ}C$, to support our earlier chemical structure model for Co species in 5 wt% $CoO_x/TiO_2$(fresh) and(spent) catalysts. Each XRD pattern for the synthesized $CoTiO_3$ and $Co_2TiO_4$ was very close to those obtained from the respective standard XRD data files. The two $CoTiO_x$ samples gave Co 2p XPS spectra consisting of very strong main peaks for Co $2p_{3/2}$ and $2p_{1/2}$ with corresponding satellite structures at higher binding energies. The Co $2p_{3/2}$ main structure appeared at 781.3 eV for the $CoTiO_3$, and it was indicated at 781.1 eV with the $Co_2TiO_4$. Not only could these binding energy values be very similar to that exhibited for the 5 wt% $CoO_x/TiO_2$(fresh), but the spin-orbit splitting(${\Delta}E$) had also no noticeable difference between the cobalt titanates and a sample of the fresh catalyst. Neither of all the $CoTiO_x$ samples were active for the wet TCE oxidation, as expected, but a sample of pure $Co_3O_4$ had a good activity for this reaction. The earlier proposed model for the surface $CoO_x$ species existing with the fresh and spent catalysts is very consistent with the XPS characterization and activity measurements for the cobalt titanates.

Preparation and Luminescent Properties of LaPO4:Re (Re=Er, Yb) Nanoparticles (희토류 이온(Er/Yb)이 도핑된 LaPO4 나노입자의 합성과 발광특성)

  • Oh Jae-Suk;Lee Tack-Hyuck;Seok Sang-Il;Jung Ha-Kyun
    • Korean Journal of Materials Research
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    • v.14 no.4
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    • pp.270-275
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    • 2004
  • Due to the luminescence by$ Er ^{ 3+}$ activator, Er-doped $LaPO_4$ powders can be applied for optical amplification materials. In this study, $LaPO_4$:Er nanoparticles were synthesized in solution system using a high-boiling coordinating solvent and their properties were investigated through various spectroscopic techniques. The nanoparticles were to take a single phase of monazite structure by a X-ray diffraction analysis and to have the 5-6 nm of particles size with narrow size distribution by a TEM. And it was confirmed by the EA and FT-IR analyses that the surfaces of nanoparticles are coordinated with the solvent molecules, which will possibly keep from agglomerating between LaPO$_4$:Er nanoparticles. In the emission spectrum of $LaPO_4$:Er nanoparticle at NIR region, on the other hand, it was measured that the emission intensity is very weak, which is due to the transition from $^4$$I_{(13/2)}$ to $^4$$I_{(15/2)}$ of $Er^{3+ }$ion. It was interpreted that the weak luminescence of $LaPO_4$:Er is originated from the hydroxyl groups adsorbed on the surfaces of the nanoparticles, because OH group acts as an efficient quencher for the $^4$$I_{(13/2)}$ \longrightarrow $^4$$I_{(15/2)}$ emission of $Er^{3+}$ activator. But the co-doping of Yb$^{3+}$ as a sensitizer in this nanoparticle results in the increase of the emission intensity at 1539 nm due to the effective energy transfer from $Yb^{3+}$ to $Er^{3+}$ . In addition, the synthesized nanoparticles exhibited good dispersibility with some polymers and effective luminescence at NIR region.n.

Synthesis and Magnetic Relaxation Properties of Paramagnetic Gd-complexes of New DTPA-bis-amides. The X-ray Crystal Structure of [Gd(L)(H2O)]·3H2O (L = DTPA-bis(4-carboxylicphenyl)amide)

  • Dutta, Sujit;Kim, Suk-Kyung;Lee, Eun-Jung;Kim, Tae-Jeong;Kang, Duk-Sik;Chang, Yong-min;Kang, Sang-Ook;Han, Won-Sik
    • Bulletin of the Korean Chemical Society
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    • v.27 no.7
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    • pp.1038-1042
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    • 2006
  • A new type of DTPA-bis-amides (L1-L4) and their Gd(III)-complexes of the type $[Gd(L)(H_2O)]{\cdot}nH_2O$ (5: L1; 6: L2; 7: L3; 8: L4) have been prepared and characterized by analytical and spectroscopic techniques. The X-ray crystal structure of 8 has been determined for structural confirmation. The coordination geometry adopts a tricapped trigonal prism geometry with L4 acting as a chelate octadentate and a water molecule in the coordination sphere. Crystals are monoclinic, $P2_1$, a = 14.468(3), b = 19.235(4), c = 13.527(2) $\AA$ $\beta$ = $107.245(3)^{\circ}$, V = 3595.2(11) $\AA^3$, Z = 4, $D_{calc}$ = 1.570. Significant increases in relaxivities are observed with 6 and 7 as compared with that of $Omniscan^{(R)}$, a commercial MR agent: R1 = 12.46 $mM^{-1}\;s^{-1}$, R2 = 8.76 $mM^{-1}\;s^{-1}$ for 6; R1 = 12.77 nm-1 s-1, R2 = 7.60 mM-1 s-1 for 7; R1 = 4.9 $mM^{-1}\;s^{-1}$, R2 = 4.8 $mm^{-1}\;s^{-1}$ for $Omniscan^{(R)}$. In the case of 5, however, both R1 and R2 are found to be lower to show 2.09 $mM^{-1}\;s^{-1}$, and 1.82 $mM^{-1}\;s^{-1}$, respectively.

[Pt(II)(cis-DACH) (DPPE)] .$2NO_3$: A Novel Class Of Platinum Complex Exhibiting Selective Cytotoxicity to Human Ovarian Carcinoma Cell Lines and Normal Kidney Cells

  • Jung, Jee-Chang;Chu, Min-Ho;Chang, Sung-Goo;Lee, Kyung-Tae;Rho, Young-Soo
    • Biomolecules & Therapeutics
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    • v.5 no.2
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    • pp.125-132
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    • 1997
  • Cisplatin, a platinum-complex, is currently one of the most effective compounds used in the treat-ment of solid tumors. However, its use is limited by severe side effects such as renal toxicity. Our platinum-based drug discovery program is aimed at developing drugs capable of diminishing toxicity and improving selective cytotoxicity. We synthesized new Pt (II) complex analogue containing 1,2-diaminocyclohexane (DACH) as carrier ligand and 1,2-bis (diphenylphosphino) ethane (DPPE) as a leaving group. Furthermore, nitrate was added to improve the solubility. A new series of [Pt(cia-DACH)(DPPE)] . $2NO_3$ (PC) was synthes-ized and characterized by their elemental analysis and by various spectroscopic techniques [infrared (IR), $_{13}$carbon nuclear magnetic resonance (NMR)] .PC demonstrated acceptable and significant antitumor activity against SKOV-3 and OVCAR-3 human ovarian carcinoma cell lines as compared with that of cisplatin. The cytotoxicity of PC in normal cells was found quite less than that of cisplatin using 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT), ($^3$H)thymidine uptake and glucose consumption tests in rabbit renal proximal tubular cells, human renal cortical cells and tissues. In conclusion, PC is considered to be more selective cytotoxicity toward human ovarian cancer cells than normal human/rabbit kidney cells.

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DNA Mediated Energy Transfer from 4',6-Diamidino-2-phenylindole to Ru(II)[(1,10-phenanthroline)2L]2+ : Effect of Ligand Structure

  • Youn, Mi-Ryung;Moon, Seok-Joon;Lee, Bae-Wook;Lee, Dong-Jin;Kim, Jong-Moon;Kim, Seog-K.;Lee, Chong-Soon
    • Bulletin of the Korean Chemical Society
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    • v.26 no.4
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    • pp.537-542
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    • 2005
  • It was proposed that Ru(II)[(1,10-phenanthroline)$_2$dipyrido[3,2-a:2',3'-c]phenazine ([Ru(phen)$_2$DPPZ]$^{2+}$)complexes and 4',6-diamidino-2-phenylindole (DAPI) simultaneously bind to poly[d(A-T)$_2$] (Biophysics. J. 2003, 85, 3865). Förster type resonance energy transfer from excited DAPI to [Ru(phen)2DPPZ]$^{2+}$ complexes was observed. In this study, we synthesized $\Delta$- and $\wedge$-[Ru(phenanthroline)$_2$dipyrido[3,2-a:2’3’c]6-azaphenazine] ([Ru(phen)$_2$DPAPZ]$^{2+}$) at which the DNA intercalating ligand DPPZ was replaced and we studied its binding properties to poly[d(A-T)$_2$] in the presence and absence of DAPI using polarized spectroscopy and fluorescence techniques. All the spectroscopic properties of the [Ru(phen)$_2$DPAPZ]$^{2+}$-poly[d(A-T)$_2$] complex were the same in the presence and absence of DAPI that blocks the minor groove of polynucleotide, suggesting both $\Delta$- and $\wedge$-[Ru(phen)$_2$DPAPZ]$^{2+}$ complexes are located at the major groove of poly[d(A-T)2]. On the other hand, in contrast with [Ru(phen)$_2$DPPZ]$^{2+}$, both $\Delta$- and $\wedge$-[Ru(phen)$_2$DPAPZ]$^{2+}$ exhibited almost twice the efficiency in the fluorescence quenching of DAPI that binds at the minor groove of poly[d(A-T)$_2$]. This observation indicates that the efficiency of the Förster type resonance energy transfer can be controlled by a small change in the chemical structure of the intercalated ligand.

Identification of anti-adipogenic withanolides from the roots of Indian ginseng (Withania somnifera)

  • Lee, Seoung Rak;Lee, Bum Soo;Yu, Jae Sik;Kang, Heesun;Yoo, Min Jeong;Yi, Sang Ah;Han, Jeung-Whan;Kim, Sil;Kim, Jung Kyu;Kim, Jin-Chul;Kim, Ki Hyun
    • Journal of Ginseng Research
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    • v.46 no.3
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    • pp.357-366
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    • 2022
  • Background: Withania somnifera (Solanaceae), generally known as Indian ginseng, is a medicinal plant that is used in Ayurvedic practice for promoting health and longevity. This study aims to identify the bioactive metabolites from Indian ginseng and elucidate their structures. Methods: Withanolides were purified by chromatographic techniques, including HPLC coupled with LC/MS. Chemical structures of isolated withanolides were clarified by analyzing the spectroscopic data from 1D and 2D NMR, and HR-ESIMS experiment. Absolute configurations of the withanolides were established by the application of NMR chemical shifts and ECD calculations. Anti-adipogenic activities of isolates were evaluated using 3T3-L1 preadipocytes with Oil Red O staining and quantitative real-time PCR (qPCR). Results: Phytochemical examination of the roots of Indian ginseng afforded to the isolation of six withanolides (1-6), including three novel withanolides, withasilolides GeI (1-3). All the six compounds inhibited adipogenesis and suppressed the enlargement of lipid droplets, compared to those of the control. Additionally, the mRNA expression levels of Fabp4 and Adipsin, the adipocyte markers decreased noticeably following treatment with 25 µM of 1-6. The active compounds (1-6) also promoted lipid metabolism by upregulating the expression of the lipolytic genes HSL and ATGL and downregulating the expression of the lipogenic gene SREBP1. Conclusion: The results of our experimental studies suggest that the withasilolides identified herein have anti-adipogenic potential and can be considered for the development of therapeutic strategies against adipogenesis in obesity. Our study also provides a mechanistic rationale for using Indian ginseng as a potential therapeutic agent against obesity and related metabolic diseases.

A Novel Acid-Base Catalyzed Sol-Gel Synthesis of Highly Active Mesoporous TiO2 Photocatalysts

  • Khan, Romana;Kim, Sun-Woo;Kim, Tae-Jeong;Lee, Hyo-Sun
    • Bulletin of the Korean Chemical Society
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    • v.28 no.11
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    • pp.1951-1957
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    • 2007
  • A new synthetic strategy based on the acid-base catalyzed sol-gel method was developed for the preparation of a series of mesoporous TiO2 nanoparticles. A key feature of the method involves a gradual change in pH (0.8- 9) during the sol-gel transition, which guarantees easy introduction of mesoporosity without relying on the well-established sonochemical or template approach. In addition, this method leads to the exclusive formation of the anatase phase stable enough to the calcination temperature up to 600 oC. The physicochemical properties of the particles in the series were characterized by various spectroscopic and analytical techniques such as wide-angle XRD, SAXRD, BET surface area, FE-SEM, TEM, FT-IR, TGA, and XPS. The photocatalytic efficiency of these materials was investigated for the oxidation of toluene under UV-irradiation. All but T-ad in the series exhibited high photocatalytic activity pushing the reaction into completion within 3 h. The reaction followed the first order kinetics, and the rate reaches as high as 3.9 × 10?2/min which exceeds the one with the commercially available Degussa P-25 by a factor of 3.2. When comparison is made among the catalysts, the reactivity increases with increase in the calcination temperature which in turn increases the crystallinity of the anatase phase, thus revealing the following rate orders: T-3 < T-4 < T-5 < T-6.

Synthesis, Characterization, and Catalytic Properties of Gp 6 Metal Complexes of 1-N,N-dimethylaminomethyl-$1^{\prime}$,2-bis(diphenylphosphino)ferrocene (FcNPP). X-ray Crystal Structure of W$(CO)_4({\eta}^2-FcNPP(O)-P,N)$

  • Kim, Tae-Jeong;Kim, Yong-Hoon;Kim, Eun-Jin;Oh, Sang-Ho;Kim, Hong-Seok;Jeong, Jong-Hwa
    • Bulletin of the Korean Chemical Society
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    • v.15 no.5
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    • pp.379-386
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    • 1994
  • Reactions of 1',2-bis(diphenylphosphino)-l-(N,N-dimethylaminomethyl)ferrocene (FcNPP) with $M(CO)_6$ (M=Cr, Mo, W) in the presence of TMNO (Trimethylamine oxide) in a stoichiometric ratio of 1 : 1.5 : 3.5 produced a series of Gp 6 metal carbonyl derivatives with a variety of coordination modes: M(CO)$_4({\eta}^2$-FcNPP-P,P) (M=Cr, Mo, W), $M(CO)_5({\eta}^1-FcNPP-P) (M=Mo, W)\;,\; M_2(CO)_9({\eta}^1\;,\;{\eta}^2-FcNPP-P,P,N) (M=Cr, Mo)\;,\;M_2(CO)_{10}({\eta}^1\;,\;{\eta}^1-FcNPP-P,P) (M=Cr, Mo, W)\;, and\;W(CO)_4({\eta}^2-FcNPP(O)-P,N)$. All these complexes were characterized by microanalytical and spectroscopic techniques. In one case, the structure of W(CO)$_4({\eta}^2$-FcNPP(O)-P,N) was determined by X-ray crystallography. Crystals are monocinic, space group P$2_{1/C}$, with a=10.147(2), b=19.902(3), c=19.821(4) ${\AA},\;{\beta}=96.88(2)^{\circ},\;V=3974(l){\AA}^3$, Z=4, and $D_{calc}=1.64 g cm^{-3}$. The geometry around the central tungsten metal is a distorted octahedron, with the nitrogen and phosphorus atoms being cis to each other. Some of these complexes exhibited catalytic activities in the allylic oxidation and epoxidation of cholesterly acetate. Other oxidation products were also formed with the different chemical yields and product distribution depending upon the ligand and the central metal.

New Azafluorenone Derivative and Antibacterial Activities of Alphonsea cylindrica Barks

  • Talip, Munirah Abdul;Azziz, Saripah Salbiah Syed Abdul;Wong, Chee Fah;Awang, Khalijah;Naz, Humera;Bakri, Yuhanis Mhd;Ahmad, Mohamad Syahrizal;Litaudon, Marc
    • Natural Product Sciences
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    • v.23 no.3
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    • pp.151-156
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    • 2017
  • A phytochemical study of Alphonsea cylindrica King (unreported) has led to the isolation of six alkaloids. The compounds were identified as kinabaline (1; azafluorenone alkaloid), muniranine (2), O-methylmoschatoline (3; oxoaporphine alkaloid), lysicamine (4), atherospermidine (5) and N-methylouregidione (6; 4, 5-dioxoaporphine alkaloid). The structures of the isolated compounds were determined based on the spectroscopic techniques and by comparison with data reported in the literature. Alkaloid 2 was isolated as a new derivative of azafluorenone while alkaloids 1, 3 - 6 were isolated for the first time from Alphonsea species. In addition, alkaloid 3 and 4 showed inhibition zone against Staphylococcus aureus, Pseudomonas aeruginosa and Bacillus cereus in disc diffusion test. The minimum inhibition concentration (MIC) values of lysicamine (4) against S. aureus, B. cereus and P. aeruginosa were found to be smaller than O-methylmoschatoline (3). Therefore, the reported antibacterial activity showed the potential of this plant as natural antibacterial agent and supported the documented traditional use of Alphonsea sp. in the treatment of diarrhea and fever.