• Title/Summary/Keyword: ChLC

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Investigation on Reaction Products From Oxidative Coupling Reactions of 1-Naphthol By Manganese Oxide (망간산화물에 의한 1-Naphthol의 산화-결합 반응에 따른 반응산물 연구)

  • Lim, Dong-Min;Lee, Doo-Hee;Kang, Ki-Hoon;Shin, Hyun-Snag
    • Journal of Korean Society of Environmental Engineers
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    • v.29 no.9
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    • pp.989-996
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    • 2007
  • In this study, abiotic transformation of 1-naphthol(1-NP) via oxidative-coupling reaction and its reaction products were investigated in the presence of Mn oxides. The reaction products were characterized for their relative polarity using solvent extraction experiment and reverse-phase HPLC, and for structure using CCMS and LC/MS, and for absorption characteristics using UV-Vis spectrometry. The reaction products present in aqueous phase were more polar than parent naphthol and comprised of 1,4-naphthoquinon(1,4-NPQ) and oligomers such as dimers and trimers. Hydrophilic component present in water phase after solvent$(CH_2Cl_2)$ extractions was identified as naphthol polymerized products having molecular weight(m/z) ranging from 400 to 2,000, and showed similar UV-Vis. absorption characteristics to that of foil fulvic acid. Transformation of 1,4-NPQ, which is non-reactive to Mn oxide, to the polymerized products via cross-coupling reaction in the presence of 1-NP was also verified. In this experimental conditions(20.5 mg/L, 1-NP, 2.5 g/L $MnO_2$, pH 5), the transformation of 1-NP into the oligomers and polymerized products were about 83% of initial 1-NP concentrations, and more than 30% of the reaction products was estimated to be water insoluble fractions, not extracted by $H_2O$ methanol. Results from this study suggest that Mn oxide-mediated treatment of naphthol contaminated soils can achieve risk reduction through the formation of oligomers md polymer precipitation.

Determination of radiolysis products in Tri-Octyl Amine by high performance liquid chromatography-mass spectrometer (HPLC-MS에 의한 Tri-Octyl Amine(TOA)의 방사선 분해산물 정량)

  • Yang, Han-Beom;Lee, Eil-Hee;Moon, Hyung-Sil
    • Analytical Science and Technology
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    • v.18 no.3
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    • pp.201-205
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    • 2005
  • Tri-octyl amine (TOA) is used in solvent extraction process for radioactive waste. This compound may be degraded to di-octyl amine (DOA), mono-octyl amine (MOA) by radioactive materials. Amount of TOA, DOA and MOA in TOA must be monitored because they production of these compounds means degradation of which leads to a decrease in the extraction yield. Retention behavior for TOA, DOA and MOA are studied with Phenomenex LUNA-$C_{18}$ ($4.6mm{\times}25cm$) analytical column and $CH_3OH:H_2O$ (50 mmol $CH_3COONH_4$) eluent by liquid chromatography. Optimum condition for these compounds is $CH_3OH:H_2O$ (50 mmol $CH_3COONH_4$) = 85 : 15 ratio. TOA, DOA and MOA compounds is well separated within 20 minute. Dynamic range is $30{\sim}160{\mu}g/mL$ for TOA, $5{\sim}100{\mu}g/mL$ for DOA and $0.1{\sim}5{\mu}g/mL$ for MOA, respectively. The detection limit are $0.1{\mu}g/mL$ for TOA, $1{\mu}g/mL$ for DOA (in SCAN mode) and $0.1{\mu}g/mL$ for MOA (in SIM mode) in this system with $20{\mu}L$ sample loop.

Quantification Analysis and Antioxidant Activity of Leejung-tang (LC-MS/MS를 이용한 이중탕(理中湯)의 정량분석 및 항산화 활성)

  • Seo, Chang-Seob;Kim, Ohn Soon;Kim, Yeji;Shin, Hyeun-Kyoo
    • Herbal Formula Science
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    • v.21 no.1
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    • pp.177-185
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    • 2013
  • Objectives : Leejung-tang (Lizhong-tang) has been used for treatment of gastrointestinal disorders in Korea. In this study, we performed quantification analysis of five marker components, liquiritin, ginsenoside Rb1, ginsenoside Rg1, glycyrrhizin, and 6-gingerol in Leejung-tang using a ultra performance liquid chromatography- electrospray ionization-mass spectrometer (UPLC-ESI-MS). In addition, we evaluated antioxidant activity of Leejung- tang. Methods : The column for separation of five constituents used a UPLC BEH C18 ($100{\times}2.1mm$, $1.7{\mu}m$) maintained at $45^{\circ}C$. The mobile phase consisted of two solvent systems, 0.1% (v/v) formic acid in H2O (A) and CH3CN (B) by gradient flow. The flow rate was 0.3 mL/min with detection at mass spectrometer. The antioxidative activities conduct an experiment on 2,2'-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) and 2,2-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging activities of Leejung-tang. Results : Calibration curves of five marker compounds were acquired with r2 values > 0.99. The amount of the five compounds in Leejung-tang were 0.07 - 0.84 mg/g. The concentration required for 50% reduction (RC50) against ABTS radical was 119.02 ug/mL. In addition, the scavenging against DPPH radical of Leejung-tang was 11.4%, 14.5%, 19.8%, 29.6%, and 49.2% at 25 ug/mL, $50{\mu}g/mL$, $100{\mu}g/mL$, $200{\mu}g/mL$, and $400{\mu}g/mL$, respectively. Conclusions : The established LC-MS/MS method will be helpful to improve quality control of Leejung-tang. In addition, Leejung-tang is a potential antioxidant therapeutic agent.

Characterization of degradation products of the Balsalazide by Mass spectrometry: Optimization of stability-indicating HPLC method for separation and quantification of process related impurities of Balsalazide

  • Chilakabattina Naga Narasimha Babu;Ch. Srinivasa Reddy;Bhagya Kumar Tatavarti;M. Radha Madhavi;Venkateswara Rao Anna
    • Analytical Science and Technology
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    • v.37 no.1
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    • pp.25-38
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    • 2024
  • The study aimed to investigate a novel approach by utilizing liquid chromatography (LC) and liquid chromatography-mass spectrometry (LC-MS) to separate, identify and characterize very nominal quantities of degradation products (DPs) of balsalazide along with its process related impurities without isolation from their reaction mixtures. The impurities along with balsalazide were resolved on spherisorb ODS2 (250×4.6 mm, 5.0 ㎛) column at room temperature using 0.2 M sodium acetate solution at pH 4.5 and methanol in the ratio of 55:45 (v/v) as mobile phase pumped isocratically at 1.0 mL/min as mobile phase and UV detection at 255 nm. The method shows sensitive detection limit of 0.003 ㎍/mL, 0.015 ㎍/mL and 0.009 ㎍/mL respectively for impurity 1, 2 and 3 with calibration curve liner in the range of 50-300 ㎍/mL for balsalazide and 0.05-0.30 for its impurities. The balsalazide pure compound was subjected to stress studies and a total of four degradation products (DPs) were formed during the stress study and all the DPs were characterized with the help of their fragmentation pattern and the masses obtained upon LC-MS/MS. The DPs were identified as 3-({4-[(E)-(4-hydroxyphenyl) diazenyl]benzoyl}amino)propanoic acid (DP 1), 4-[(E)-(4-hydroxyphenyl)diazenyl] benzamide (DP 2), 5-[(E)-(4-carbamoylphenyl)diazenyl]-2-hydroxybenzoic acid (DP 3) and 3-({4-[(E)-phenyldiazenyl]benzoyl}amino)propanoic acid (DP 4). Based on findings, it was concluded that, the proposed method was successfully applicable for routine analysis of balsalazide and its process related impurities in pure drug and formulations and also applicable for identification of known and unknown impurities of balsalazide.

Liquid Crystal Aligning Capabilities in the Photoaligned TN-Cell on Blending Photopolymer (복합 광폴리머 표면을 이용한 장배향 TN 셀의 액정배향 특성)

  • Hwang, Jeoung-Yeon;Jo, Yong-Min;Seo, Dae-Shik;Suh, Dong-Hack
    • Proceedings of the KIEE Conference
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    • 2001.11a
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    • pp.178-181
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    • 2001
  • The electro-optical (EO) characteristics for the twisted-nematic (TN)-liquid crystal display (LCD) photo-aligned with polarized UV exposure on various blending photopolymer surfaces were investigated. Excellent LC alignment and voltage-transmittance (V-T) characteristics for TN-LCD photo-aligned with polarized UV exposure of normal incidence on the blending Photopolymer (polyimide (PI) + PM4Ch (poly(4-methacryloyloxy chalcone))) surface containing chalcone group can be achieved. The EO performances of the TN-LCD photo-aligned on the blending photopolymer can be improved due to the photosensitivity by long side chain of the photopolymer.

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Laser -addressing Electronic Paper

  • Chen, Heng-Yin;Lu, Shao-Chuan;Chen, Shang-Chia;Lin, Hsuan-Kai;Liu, Sung-Ho;Chen, Chun-Ming;Liang, Chao-Chiun
    • 한국정보디스플레이학회:학술대회논문집
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    • 2008.10a
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    • pp.175-178
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    • 2008
  • A new laser-addressing method is proposed in this paper. With the characteristic of high power and small spot size, simple structure electronic paper can be addressed only by laser source, and high quality image with 300dpi resolution can be easily achieved.

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Electro-optical Characteristics of the TN Cell Photo-aligned on the Blending Photopolymer Surfaces (복합 광폴리머 표면을 이용한 광배향 TN 셀의 전기 광학 특성)

  • 황정연;서대식
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.14 no.7
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    • pp.600-605
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    • 2001
  • The electro-optical (EO) performances for the twisted-nematic (TN)-liquid crystal display (LCD) photo-aligned with polarized UV exposure on various blending photopolymer surfaces were investigated. Excellent LC alignment and voltage-transmittance (V-T) characteristics for TN-LCD photo-aligned with polarized UV exposure of normal incidence on the blending photopolymer (polyimide (PI) +PM4Ch(poly(4-methacryloyloxy chalcone))) surface containing chalcone group can be achieved. The EO performances for the TN-LCD photo-aligned on the blending photopolymer can be improved due to the photosensitivity by long side chain of the photopolymer.

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Pretilt Angel Generation and Alignment Stability for Nematic Liquid Crystal Using a Photodimerization Method (광중합법을 이용한 네마틱액정의 배향 안정성 및 프리틸트각의 발생)

  • 황정연;서대식;김재형;한은주
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.14 no.4
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    • pp.336-340
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    • 2001
  • We have investigated the generation of pretilt angle and alignment stability for a nematic liquid crystal (NLC) with obliquely polarized UV exposure on the three kinds of photo-polymer. High pretilt angle of the NLC was obtained by polarized UV exposure on a PM4Ch surface for 1 min. But, the low pretilt angle of he NLC on a PVCi surface was observed. The pretilt angle generated is attributed ot the photosensitivity by the long side chaining of photo-polymer. Also, a good thermal stability of the three kinds of photo-polymer were obtained by thermogravimetric analysis (TGA) measurement until 300$^{\circ}C$. Finally, the good LC aligning capabilities using the photodimerization method were observed by annealing-treatment until 150$^{\circ}C$.

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Grignard Coupling Reaction of Bis(chloromethyl)diorganosilanes with Dichloro(diorgano)silanes: Syntheses of 1,3-Disilacyclobutanes

  • 조연석;유복렬;안삼영;정일남
    • Bulletin of the Korean Chemical Society
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    • v.20 no.4
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    • pp.427-430
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    • 1999
  • The Grignard coupling reaction of bis(chloromethyl)diorganosilanes [(ClCH2)2SiR1R2: R1 = R2 = Me, la; R1 = Me, R2 = Ph, lb; R1 = R2 = Ph, lc] with diorganodichlorosilanes [(Cl2SiR3R4: R3 = R4 = Me, 2a; R3 = Me, R4 = Ph, 2b; R3 = R4 = Ph, 2c] at THE reflux temperature gave the intermolecular C-Si coupling product of 1,1,3,3-tetraorgano-1,3-disilacyclobutanes 3a-f in poor to moderate yields ranging from 7% to 50% along with polydiorganosilapropanes. The cyclization reaction of la-c with methyl-substituted dichlorosilanes 2a, b gave 1,3-disilacyclobutanes 3a-c, e, d in moderate yields (42-50%), while the same reaction with dichlorodiphenylsilane (2c) to 1,3-disilacyclobutanes 3d, f resulted in low yield (7-18%) probably due to the steric hindrance of two-phenyl groups on the silicon of 2c.

Diagnostic and Prognostic Roles of Serum Osteopontin and Osteopontin Promoter Polymorphisms in Hepatitis B-related Hepatocellular Carcinoma

  • Chimparlee, Nitinan;Chuaypen, Natthaya;Khlaiphuengsin, Apichaya;Pinjaroen, Nutcha;Payungporn, Sunchai;Poovorawan, Yong;Tangkijvanich, Pisit
    • Asian Pacific Journal of Cancer Prevention
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    • v.16 no.16
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    • pp.7211-7217
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    • 2015
  • Background: The aims of this study were to evaluate the diagnostic and prognostic roles of serum osteopontin (OPN) and single nucleotide polymorphisms (SNPs) in the OPN promoter in patients with hepatitis B-related hepatocellular carcinoma (HCC). Materials and Methods: Four groups were studied, which included 157 patients with HCC, 73 with liver cirrhosis (LC) and 97 with chronic hepatitis (CH), along with 80 healthy subjects. Serum OPN and alpha-fetoprotein (AFP) levels were measured. The SNPs -66 T/G, -156 G/${\Delta}G$ and -433 C/T within the OPN promoter were determined by direct sequencing. Results: Serum OPN levels were significantly higher in patients with HCC than in the other groups. Area under receiver operating characteristics curves in distinguishing HCC from chronic liver disease (CLD; CH and LC) were 0.782 (95% CI; 0.729-0.834) for OPN and 0.888 (95% CI; 0.850-0.927) for AFP. Using the optimal cut-off value (70 ng/mL), OPN had sensitivity and specificity of 72% and 71%, respectively. Serum OPN was superior to AFP in detecting early-stage HCC (68% vs. 46%). A combination of both markers yielded an improved sensitivity for detecting early HCC to 82%. A high OPN level was significantly correlated with advanced BCLC stage and was an independent prognostic factor for HCC. The SNPs -156 and -443 were associated with susceptibility to HCC, but were not related to overall survival. Conclusions: Serum OPN is a useful diagnostic and prognostic marker for HCC. The combined use of serum OPN and AFP improved the diagnosis of early HCC. Genetic variation in the OPN promoter is associated with the risk, but not the prognosis of HCC.