• Title/Summary/Keyword: spectroscopic method

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Crystal Growth of $Cr:Al_2O_3$ and $Ti:Al_2O_3$ by Czochralski Technique (용액인상법에 의한 $Cr:Al_2O_3$$Ti:Al_2O_3$ 단결정 육성)

  • Yu, Yeong-Mun;Lee, Yeong-Guk;Park, Ro-Hak
    • Korean Journal of Crystallography
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    • v.6 no.1
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    • pp.1-13
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    • 1995
  • Cr:A12O3 and Ti:A12O3 single crystals were grown by Czochralski method, and the effects of crystal growth parameters such as pulling rate, rotation rate, dopant and growth atmosphere on crystal quality were investigated. And spectroscopic properties including lasing efficiency were also measured. Single crystals, sized of 20mm in diameter and 100-135mm in length, were successfully grown from the seed of <001> direction. With the doping level of 0.5w/o Cr2O3, pulling rate 2.0mm/hr, rotation rate of 30rpm and inert atmosphere by nitrogen gas, high quality crystals of Cr:A12O3 were grown. While in case of Ti:A12O3 crystals, high quality crystals were grown under the conditions of the doping level of 0.25w/o TiO2, pulling rate of 1.5mm/hr, rotation rate of 30rpm and reducing atmosphere by hydrogen - nitrogen mixed gas. It was confirmed that Cr3+ ion which maintains its ionoc valence during growth easily de-bubbled than Ti4+ ion which changes its valence, Fe3+ ion also has do-bubbling effect to Ti:A12O3 crystal and the reducing atmosphere by 90% N2 - 10% H2 mixed gas gave effective result on the changing of Ti4+ to Ti3+ and de-bubbling. As a result of spectroscopic measurements of Cr:A12O3 crystal, 4A2 →4F2 and 4F1 absorption transitions and E →4A2(R1) and 2A →4A2(R2) fluorenscence transitions were confirmed. And it was measured that wavelengths of laser R1 and R2 transitions were 696±5nm and 692±5nm respectively, line width of these transitions were 12A, and life-time of fluorenscence was 152μsec. In case of Ti:A12O3 crystals, it was confirmed that absortion transition of 4T2→4E and fluorescence transition of 4E→4T2 with wide range of 650-1050nm was occured. And 147μsec of life-time of fluorescence, 125.4 of figure of merit and 9% of laser efficience were also measured.

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Tautomerism and Alkylation of 5-Amino-2H-1,2,4-thiadiazoline-3-one (5-Amino-2H-1,2,4-thiadiazoline-3-one의 토토머화 현상과 알킬화 반응)

  • Cho, Nam Sook;Park, Young Cheol;Ra, Do Young;Kang, Sungkwon
    • Journal of the Korean Chemical Society
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    • v.39 no.7
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    • pp.564-571
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    • 1995
  • 5-Amino-2H-1,2,4-thiadiazoline-3-one has been prepared from 2-thiobiuret through a oxidative cyclization under basic hydrogen peroxide condition. Lactam-lactim tautomerism of 5-amino-2H-1,2,4-thiadiazoline-3-one has been examined by spectroscopic methods and ab initio molecular orbital calculation. These results were shown that 5-amino-2H-1,2,4-thiadiazoline-3-one exists as lactam form. Reaction conditions for alkylating 5-amino-2H-1,2,4-thiadiazoline-3-one with alkyl halides in the presence of various bases were studied in DMF and $H_2O$-THF two phase system. $Li_2CO_3$ base in DMF method gave best result in this investigation. The alkylation has been taken place at N-2 position. The identification of the product is confirmed by spectral data of IR, $^1H$ NMR and $^13C$ NMR and the comparison of authentic sample, 5-amino-2-methyl-1,2,4-thiadiazolidine-3-one, obtained from the oxidative cyclization of 5-methyl-2-thiobiuret.

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Antitumor Activity and Nephrotoxicity of the Novel Platinum(II) Coordination Complex (새로운 Platinum (II) Complex [Pt (II)(trans-d-dach)(DPPE)] $(NO_3)_2$의 항암효과 및 신독성에 관한 연구)

  • Jung Jee-Chang;Lee Moon-Ho;Chang Sung-Goo;Rho Young-Soo
    • The Korean Journal of Pharmacology
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    • v.31 no.1 s.57
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    • pp.103-114
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    • 1995
  • Platinum coordination complexes are currently one of the most compounds used in the treatment 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 antitumor activity. 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(trans-ddach)(DPPE).$2NO_3(PC)$ was synthesized and characterized by their elemental analysis and by various spectroscopic techniques [infrared (IR), $^{13}carbon$ nuclear magnetic resonance (NMR)]. PC demonstrated acceptable antitumor activity aganist P388, L-1210 lymphocytic leukemia cells and SK=OV3 human ovarian adenocarcinoma cells, and significant. activity as compared with that. cisplatin. The toxicity of PC was found quite less than thar of cisplatin using MTT, $[^3H]$ thymidine uptake and glucose consumption tests in rabbit proximal tubule cells, human kidney cortical cells and human renal cortical tissues. Based on these results, this novel platinum compound represent a valuable lead in the development of a new anticancer chemotherapeutic agent capable of improving antitumor activity and low toxicity.

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Separation and Elution Behaviors of Some Metal-2-hydroxyarylazopyrazolone Chelates by Reversed Phase High Performance Liquid Chromatography (I) (역상 액체 크로마토그래피에 의한 금속-2-hydroxyarylazopyrazolone 유도체 킬레이트의 용리거동 및 동시분리에 관한 연구 (I))

  • Lee, Chang-Heon;Kang, Chang-Hee;Kim, Eun-Kyung;Lee, Won
    • Analytical Science and Technology
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    • v.7 no.1
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    • pp.103-114
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    • 1994
  • The elution behaviors of Ni(II), Cu(II), Co(II), and Cr(II) in 1-phenyl-3-methyl-4(2-hydroxy-5-X-phenylazo)-5-pyrazolone, [Pm(2-OH)(5-X)PaPz](X=H, $CH_3$, $NO_2$, Cl) chelates have been studied by reversed phase HPLC. Thirteen metal-[Pm(2-OH)(5-X)PaPz] chelates were prepared and characterized by UV, IR, MS, and ICP spectroscopic methods. These metal-2-hydroxyarylazopyrazolone chelates were successfully separated on Novapak-$C_{18}$ column using methanol/water mixtures as a mobile phases. It was found that the chelates were eluted properly in an acceptable range of the capacity factor value($0{\leq}log\;k^{\prime}{\leq}1$). The dependence of the capacity factor(log k') on the volume fraction of water in the binary mobile phase showed a good linearity. Also, there was a good linear dependence of the capacity factor on the liquid-liquid extraction distribution ratio($D_c$) in methanol-water/n-pentadecane extraction system by the batch method. It suggested that the retention of the chelates in the reverse phase liquid chromatographic system be largely due to the solvophobic effect.

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Real-time monitoring for blending uniformity of trimebutine CR tablets using near-infrared and Raman spectroscopy (근적외분광분석법과 라만분광분석법을 이용한 트리메부틴말레인산 서방정의 혼합 과정 모니터링)

  • Woo, Young-Ah
    • Analytical Science and Technology
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    • v.24 no.6
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    • pp.519-526
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    • 2011
  • Chemometrics using near-infrared (NIR) and Raman spectroscopy have found significant uses in a variety quantitative and qualitative analyses of pharmaceutical products in complex matrixes. Most of the pharmaceutical can be measured directly with little or no sample preparation using these spectroscopic methods. During pharmaceutical manufacturing process, analytical techniques with no or less sample preparation are very critical to confirm the quality. This study showed NIR and Raman spectroscopy with principal component analysis (PCA) was very effective for the blending processing control. It is of utmost importance to evaluate critical parameters related to quality of products during pharmaceutical processing. The blending is confirmed by off-line determination of active pharmaceutical ingredient (API) by a conventional method such as high performance liquid chromatography (HPLC) and UV spectroscopy. These analytical methods are time-consuming and ineffective for real time control. This study showed the possibility for the determination of blend uniformity end-point of CR tablets with the use of both NIR and Raman spectroscopy. The samples were acquired from six positions during blending processing with U-type blender from 0 to 30 min. Using both collected NIR and Raman spectral data, principal component analysis (PCA) was used to follow the uniformity of blending and finally determine the end-point. The variation of homogeneity of six samples during blending was clearly found and blend uniformity end-point was successfully confirmed in the domains of principal component (PC) scores.

NMR Studies on the Structure of Human Annexin I

  • Han, Hee-Yong;Bang, Keun-Su;Na, Doe-Sun;Lee, Bong-Jin
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1996.04a
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    • pp.182-182
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    • 1996
  • Annexin I is a member of the annexin family of calcium dependent phospholipid binding proteins and has anti-inflammatory activity by inhibiting phospholipase A$_2$ (PLA$_2$). Recent X-ray crystallographic study of annexin I identified six Ca$\^$2+/ binding bites, which was different types (type II, III) from the well-known EF-hand motif (type I). In this work, the structure of annexin I was studied at atomic level by using $^1$H, $\^$15/N and $\^$l3/C NMR(nuclear magnetic resonance) spectroscopy, and the effect of Ca$\^$2+/ binding on the structure of annexin I was studied, and compared with that of Mg$\^$2+/ binding, When Ca$\^$2+/ was added to annexin I, NMR peak change was occured in high- and low-field regions of $^1$H-NMR spectra. NMR peak change by Ca$\^$2+/ binding was different from that by Mg$\^$2+/ binding. Because annexin I is a larger protein with 35 kDa molecular weight, site-specific (amide-$\^$15/N, carbonyl-$\^$l3/C) labeling technique was also used. We were able to detect methionine, tyrosine and phenylalanine peaks respectively in $\^$13/C-NMR spectra, and each residue was able to be assigned by the method of doubly labeling annexin I with [$\^$13/C] carbonyl-amino acid and [$\^$15/N] amide-amino acid. In $\^$l3/C-NMR spectra of [$\^$13/C] carbonyl-Met labeled annexin I, we observed that methionine residues spatially located near Ca$\^$2+/ binding Sites Were Significantly effected by Ca$\^$2+/ binding. From UV spectroscopic data on the effect of Ca$\^$2+/ binding, we knew that Ca$\^$2+/ binding sites of annexin I have cooperativity in Ca$\^$2+/ binding. The interaction of annexin I with PLA$_2$ also could be detected by using heteronuclear NMR spctroscopy. Consequently, we expect that the anti-inflammatory action mechanism of annexin I may be a specific protein-protein interaction. The residues involved in the interaction with PLA$_2$ can be identified as active site by assigning NMR peaks effected by PLA$_2$ binding.

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PHOTOELECTRIC OBSERVATIONS AND UBVRI LIGHT CURVES ANALYSIS OF ALGOL (Algol의 광전측광관측과 UBVRI 광도곡선의 분석)

  • 정장해;이용삼;임조령;양감징
    • Journal of Astronomy and Space Sciences
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    • v.10 no.2
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    • pp.123-145
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    • 1993
  • UBVRi photometry of Algol was carried out from December of 1988 to March of 1991 at Chungbuk National University Observatory and a total of 3465 observations in U, B, V, R, I were obtained. Three times of primary minimum light of JDH el 2447898.0938, JEH el 2448265.1205 and JDH el 2448288.0598, and two secondary minimum light of JDH el 2447808.1014 and JDH el 2448275.146 were determined from our observations. We analyzed simultaneously the UBVRI light curves of the Algol system with the Wilson-Devinney method for the determination of the photometric parameters. Indivisual masses for the 3 components of Algol are derived as $m_1$=3.36, $m_2$=0.76, $m_3$=1.6 in solar mass and radii as $R_1$=2.97, $R_2$=0.76 in solar radinus using i=$82.{\circ}47$, q=0.227, $r_1$=0.2102, $r_2$=0.2512 of our solution and some parameters of the spectroscopic solution of Hill et al. (1971). Our results is simiar to those reported by Kim (1989). The temperature of Algol C, $T_3$=8800 was obtained by means of fitting $l_1$, $l_2$, and $l_3$ of five colors to Planckian curve, and $R_3$=$1.6R_\odot$ is derived from its result. It is believed that its semidetached configuration of Algol A and B is the consequence of case B mass transfer. According to its location in a mass-radius diagram. Algol b may have evolved significantly in its Hburnning phase.

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The Study of the Characteristic of Ti Thin Film Using Small Magnetron Sputtering Method for Sunglass Lens (소형 Magnetron sputtering 방법에 의한 썬글라스 렌즈용 Ti 박막의 특성연구)

  • Park, Moonchan;Jung, Boo Young;Lee, Jong Geun;Joo, Kyung Bok;Lee, Wha Ja
    • Journal of Korean Ophthalmic Optics Society
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    • v.13 no.1
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    • pp.59-63
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    • 2008
  • Purpose: Ti thin films were deposited on slide glass and CR-39 lenses using small magnetron sputtering apparatus to of Ti thin films. Methods: The thickness of Ti thin films were measured by cross section SEM, the transmittance and reflectance of them were obtained using spectrophotometer, the refractive index and extinction of them were obtained from VASE data. Results: The transmittances of Ti thin films with 60 nm, 120 nm, 140 nm thickness were a little change within the visual region from 400 nm to 750 nm, but were increased a little amount at near 400 nm. The transmittance of 60 nm, 120 nm, 140 nm Ti thickness in d-line was 30%, 25%, 20%, respectively. Also, it was shown that the refractive indices and extinction coefficients of the Ti thin films obtained from VASE were similar to those of Ti thin film offered macleod program. Conclusions: Ti films on CR-39 with these transmittances were available for sunglass lens. It was indicated that the refractive indices and extinction coefficients of the Ti thin films were decreased with the thickness of Ti thin film, for the thickness of Ti thin films was due to very thin.

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A New Class of Platinum (II) Complexes [Pt (trans-1-daeh) (DPPP)] $2NO_3$ and [Pt (trans-1-daeh)(DPPE)] $2NO_3$ Exhibiting Antitumor Activity and Nephrotoxieity (새로운 Platinum (II) Complex ([Pt (II)(trans-1-dach)(DPPP)] $(NO_3)_2$와 [Pt (II)(trans-1-dach)(DPPE)] $(NO_3)_2$의 항암효과 및 신독성에 관한연구)

  • Jung, Jee-Chang;Yoon, Chin-Hee;Chang, Sung-Goo;Lee, Kyung-Tae;Rho, Young-Soo
    • The Korean Journal of Pharmacology
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    • v.29 no.2
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    • pp.283-295
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    • 1993
  • Pt-complexes is currently one of the most compounds used in the treatment of solid tumors. However, its used 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 antitumor activity. We synthesized new Pt (II) complex analogues containing 1, 2-diaminocyclohexane (dach) as carrier ligand and 1, 3-bis (diphenylphosphino) propane (DPPP)/1,2-bis (diphenylphosphino) ethane (DPPE) as a leaving group. Furthermore, nitrate was added to improve the solubility. A new series of (KHPC-001) [Pt (trans-1-dach)(DPPP)] $2NO_3$ and (KHPC-002) [Pt (trans-1-dach)(DPPE)] $2NO_3$ were synthesized and characterized by their elemental analysis and by various spectroscopic techniques [infrared (IR), $^{13}carbon$ nuclear magnetic resonance (NMR)]. KHPC-001 and KHPC-002 demonstrated acceptable antitumor activity aganist P-388, L-1210 lymphocytic leukemia cells and significant activity as compared with that of cisplatin. The toxicity of KHPC-001 and KHPC-002 was found quite less than that of cisplatin using MTT, $[^3H]$ thymidine uptake and glucose consumption tests in rabbit proximal tubule cells and human kidney cortical cells.

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Effect of Lidocaine-HCl on Microviscosity of Phosphatidylcholine Model Membrane

  • Chung, In-Kyo;Kim, Inn-Se;Choi, Chang-Hwa;Cho, Goon-Jae;Kim, Jin-Bom;Son, Woo-Sung;Jang, Hye-Ock;Yun, Il
    • The Korean Journal of Physiology and Pharmacology
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    • v.4 no.3
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    • pp.243-251
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    • 2000
  • In order to provide a basis for studying the molecular mechanism of pharmacological action of local anesthetics and to develop a fluorescence spectroscopic method which can detect the microviscosity of native and model membranes using intramolecular excimerization of 1,3-di(l-pyrenyl)propane (Py-3-Py), we examined the effect of lidocaine HCl on the microviscosity of model membranes of phosphatidylcholine fraction extracted from synaptosomal plasma membrane vesicles (SPMVPC). The excimer to monomer fluorescence intensity ratio (I'/I) of Py-3-Py in liquid paraffin was a simple linear function of $T/{\eta}.$ Based on this calibration curve, the microviscosity values of the direct probe environment in SPMVPC model membranes ranged from $234.97{\pm}48.85$ cP at $4^{\circ}C$ to %19.21{\pm}1.11$ cP at $45^{\circ}C.$ At $37^{\circ}C,$ a value of $27.25{\pm}0.44$ cP was obtained. The lidocaine HCl decreased the microviscosity of SPMVPC model membranes in a concentration-dependent manner, with a significant decrease in microviscosity value by injecting the local anesthetic even at the concentration of 0.5 mM. These results indicate that the direct environment of Py-3-Py in the SPMVPC model membranes is significantly fluidized by the lidocaine HCl. Also, the present study explicitly shows that an interaction between local anesthetics and membrane lipids is of importance in the molecular mechanism of pharmacological action of lidocaine HCl.

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