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Study on Solid Phase Extraction and Spectrophotometric Determination of Nickel in Waters and Biological Samples

  • Hu, Qiu-Fen;Yang, Guan-Gyu;Huang, Zhang-Jie;Yin, Jia-Yuan
    • Bulletin of the Korean Chemical Society
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    • v.25 no.4
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    • pp.545-548
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    • 2004
  • A sensitive, selective and rapid method for the determination of nickel based on the rapid reaction of nickel(II) with QADMAA and the solid phase extraction of the Ni(II)-QADMAA chelate with $C_{18}$ membrane disks has been developed. In the presence of pH 6.0 buffer solution and sodium dodecyl sulfonate (SDS) medium, QADMAA reacts with nickel to form a violet complex of a molar ratio of 1 : 2 (nickel to QADMAA). This chelate was enriched by solid phase extraction with $C_{18}$ membrane disks. An enrichment factor of 50 was obtained by elution of the chelates form the disks with the minimal amount of isopentyl alcohol. The molar absorptivity of the chelate was $1.32{\times}10^5L\;mol^{-1}cm^{- 1}$ at 590 nm in the measured solution. Beer's law was obeyed in the range of 0.01-0.6 ${\mu}$g/mL. This method was applied to the determination of nickel in water and biological samples with good results.

Study on Solid Phase Extraction and Spectrophotometric Determination of Vanadium with 2-(2-Quinolylazo)-5-Diethylaminophenol

  • Hu, Qiu-Fen;Yang, Guan-Gyu;Huang, Zhang-Jie;Yin, Jia-Yuan
    • Bulletin of the Korean Chemical Society
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    • v.25 no.2
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    • pp.263-266
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    • 2004
  • A sensitive, selective and rapid method has been developed for the determination ${\mu}$g/L level of vanadium ion based on the rapid reaction of vanadium(V) with 2-(2-quinolylazo)-5-diethylaminophenol (QADEAP) and the solid phase extraction of the colored chelate with $C_{18}$ cartridge. The QADEAP reacts with V(V) in the presence of citric acid-sodium hydroxide buffer solution (pH = 3.5) and cetyl trimethylammonium bromide (CTMAB) medium to form a violet chelate of a molar ratio 1 : 2 (V(V) to QADEAP). This chelate was enriched by solid phase extraction with $C_{18}$cartridge and the enrichment factor of 50 was obtained by elution of the chelates from the cartridge with ethanol. The molar absorptivity of the chelate is $1.28 {\times}10^5L\;mol^{-1}cm^{-1}$ at 590 nm in the measured solution. Beer's law is obeyed in the range of 0.01-0.6 ${\mu}$g/mL. The detection limit is 0.04 ${\mu}$g/L in the original samples. This method was applied to the determination of vanadium(V) in water and biological samples with good results.

A 100 kDa Protein Binding to bHLH Family Consensus Recognition Sequence of RAT p53 Promoter

  • Lee, Min-Hyung;Park, Sun-Hee;Song, Hai-Sun;Lee, Kyung-Hee;Park, Jong-Sang
    • BMB Reports
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    • v.30 no.3
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    • pp.205-210
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    • 1997
  • p53 tumor suppressor plays an important role in the regulation of cellular proliferation. To identify proteins regulating the expression of p53 in rat liver, we analyzed p53 promoter by electrophoretic mobility shift assay (EMSA) and DNase I footprinting assay. We found that a protein binds the sequence CACGTG, bHLH consensus sequence in rat p53 promoter. Southwestern blotting analysis with oligonucleotides containing this sequence shows that the molecular weight of the protein is 100 kDa. This size is not compatible with the bHLH family such as USF or c-Myc/Max which is known to regulate the expression of the human and mouse p53 gene. Therefore this 100 kDa protein may be a new protein regulating basal transcription of rat p53. We purified this 100 kDa protein through sequence-specific DNA affinity chromatogaphy.

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2D-QSAR and HQSAR on the Inhibition Activity of Protein Tyrosine Phosphatase 1B with Oleanolic Acid Analogues

  • Chung, Young-Ho;Jang, Seok-Chan;Kim, Sang-Jin;Sung, Nack-Do
    • Journal of Applied Biological Chemistry
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    • v.50 no.2
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    • pp.52-57
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    • 2007
  • Quantitative structure-activity relationships (QSARs) on the inhibition activities by oleanolic acid analogues (1-19) as a potent inhibitor against protein tyrosine phosphatase-1B were studied quantitatively using 2D-QSAR and HQSAR methodologies. The inhibition activity was dependent on the variations of $R_{4-}$substituent, and as shown in 2D-QSAR model ($r^2=0.928$), it has a tendency to increase as the negative Randic Indice (RI) goes up. The size of the molecular fragments used in HQSAR varied from five to eight. The fragment distinctions had the best statistic value, whose predictability is $q^2=0.785$ and correlation coefficient is $r^2=0.970$, on condition of connections. From the atomic contribution maps, the factor that contributes to the inhibition activities is the $C_{15}{\sim}C_{17}$ bond in the D ring. From the analysis result of these two the models, the structural distinctions and descriptors that contribute to the inhibition activities were obtained.

Evaluation of geochemical processes affecting groundwater chemistry in Namwon, Korea

  • Kim, Kang-Joo;Natarajan Rajmohan;Kim, Hyung-Jung;Kim, Suk-Hwi;Hwang, Gab-Soo;Cho, Min-Joe;Lee, Sang-Ho
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2004.09a
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    • pp.334-337
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    • 2004
  • Groundwater chemistry in Namwon area, Korea, was investigated to understand the contribution of geochemical processes on groundwater chemistry. For this study, a total of 279 groundwater samples were collected from 93 wells distributed over the study area. Higher concentrations of major ions are generally encountered in the shallow alluvial wells, suggesting that these chemicals are originated from the surface contamination sources. Mass balance analysis based on reaction stoichiometry reveals that the water chemistry is regulated by three major chemical processes: weathering of silicate/ carbonate minerals, input of C1/SO$_4$ salts, and nitrate generating processes. The results show that mineral weathering is the most dominating factor regulating the groundwater chemistry. However, the groundwaters with the higher salt concentration indicate the larger mineral weathering effect, suggesting that some part of the mineral weathering effect is also associated with the anthropogenic activities such as limes applied to the cultivated lands, carbonates (CaCO$_3$) in the cement materials.

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Sorption of Chromium Ions from Aqueous Solution onto Chemically Activated Carbons Developed from Maize Cobs

  • Youssef, A.M.;El-Nabarawy, Th.;Shouman, Mona A.;Khedr, S.A.
    • Carbon letters
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    • v.9 no.4
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    • pp.275-282
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    • 2008
  • Chemically activated carbons were prepared from maize cobs, using phosphoric acid of variable concentration. The textural parameters of the activated carbons were determined from the nitrogen adsorption isotherms measured at 77 K. The chemistry of the carbon surface was determined by measuring the surface pH, the pHPZC and the concentration of the carbon - oxygen groups of the acid type on the carbon surface. Kinetics of Cr(VI) sorption/reduction was investigated at 303 K. Two processes were investigated in terms of kinetics and equilibrium namely; Cr(VI) removal and chromium sorption were studied at various initial pH (1-7). Removal of Cr(VI) shows a maximum at pH 2.5. At pH<2.5, sorption decreases because of the proton competition with evolved Cr(III) for ion exchange sites. The decrease of sorption at pH>2.5 is due to proton insufficiency and to the decrease of the extent of Cr(VI) reduction. The chemistry of the surface of activated carbon is an important factor in determining its adsorption capacity from aqueous solutions particularly when the sorption process involves ion exchange.

Synthesis and Application of New Ru(II) Complexes for Dye-Sensitized Nanocrystalline TiO2 Solar Cells

  • Seok, Won-K.;Gupta, A.K.;Roh, Seung-Jae;Lee, Won-Joo;Han, Sung-Hwan
    • Bulletin of the Korean Chemical Society
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    • v.28 no.8
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    • pp.1311-1316
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    • 2007
  • To develop photo-sensitizers for dye-sensitized solar cells (DSCs) used in harvesting sunlight and transferring solar energy into electricity, we synthesize novel Ru(II) polypyridyl dyes and describe their characterization. We also investigate the photo-electrochemical properties of DSCs using these sensitizers. New dyes contain chromophore unit of dafo (4,5-diazafluoren-9-one) or phen-dione (1,10-phenanthroline-5,6-dione) instead of the nonchromophoric donor unit of thiocyanato ligand in cis-[RuII(dcbpy)2(NCS)2] (dcbpy = 4,4'-dicarboxy- 2,2'-bipyridine) coded as N3 dye. For example, the photovoltaic data of DSCs using [RuII(dcbpy)2(dafo)](CN)2 as a sensitizer show 6.85 mA/cm2, 0.70 V, 0.58 and 2.82% in short-circuit current (Jsc ), open-circuit voltage (Voc), fill factor (FF) and power conversion efficiency (Eff), which can be compared with those of 7.90 mA/ cm2, 0.70 V, 0.53 and 3.03% for N3 dye. With the same chelating ligand directly bonded to the Ru metal in the complex, the CN ligand increases the Jsc value by double, compared to the SCN ligand. The extra binding ability in these new dyes makes them more resistant against ligand loss and photo-induced isomerization within octahedral geometry.

Continuous Preconcentration of Sn2+/Sn4+ by the On-line Sulfide Precipitation-Dissolution

  • Yeon, Pyung-Heum;Yoon, Young-Suk;Oh, Se-Woung;Nam, Sang-Ho;Par, Yong-Nam
    • Bulletin of the Korean Chemical Society
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    • v.25 no.8
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    • pp.1156-1160
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    • 2004
  • The technique of an on-line preconcentration by the direct sulfide precipitation has been developed. Sn was homogeneously precipitated by sulfide, which was generated in situ from the hydrolysis of thioaceteamide. Precipitate was collected on a filter in the line and dissolved out instantaneously by KOH to be sent to an ICP. The enrichment factor was 4 with the sampling speed of 15/hr for 1.0 mL of sample. It was increased to more than 40 times when the sampling volume was increased to 10 mL with the sampling speed of 5/hr. $Sn^{2+}/Sn^{4+}$ could be separately determined with the on-line precipitation technique. The method was applied to the analysis of NIST SRM 1566 Oyster sample and yielded good agreement with the certified value.

Chirality Conversion of Dipeptides in the Schiff Bases of Binol Aldehydes with Multiple Hydrogen Bond Donors

  • Park, Hyun-Jung;Hong, Joo-Yeon;Ham, Si-Hyun;Nandhakumar, Raju;Kim, Kwan-Mook
    • Bulletin of the Korean Chemical Society
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    • v.30 no.2
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    • pp.409-414
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    • 2009
  • Novel binol aldehydes derivatized at 2' hydroxy position with both uryl and acetamide groups (2), and diuryl groups (3) have been synthesized. Both were designed for streospecific binding and chirality conversion of general dipeptides with support of multiple hydrogen bonding donor sites in the receptors. The receptors, 2 and 3, converted the chirality of N-terminal amino acids of peptides such as Ala-Gly, Met-Gly, Leu-Gly and His-Gly with stereoselectivity on D-form over L-form. The stereoselectivity ratios were in the range of 5-11, somewhat higher than those of the binol receptor with mono uryl group (1). The DFT calculation at the B3LYP/6-31G$^*$//MPWB1K/6-31G$^*$ level revealed that 3-D-Ala-Gly was 2.2 kcal/mol more stable than 3-L-Ala-Gly. The considerable steric hindrance between the methyl group of the alanine and the imine CH moiety of the receptor seems to be the main contributing factor for the thermodynamic preference.

An NMR Study on the Conformation of Substance P in Acidic Bicelles

  • Baek, Seung-Bin;Lim, Sung-Chul;Lee, Hyeong-Ju;Lee, Hee-Cheon;Kim, Chul
    • Bulletin of the Korean Chemical Society
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    • v.32 no.10
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    • pp.3702-3706
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    • 2011
  • The conformation of a neuropeptide, substance P (SP), in isotropic (q = 0.5) acidic bicelles was investigated using two-dimensional NMR techniques. By the nuclear Overhauser effect (NOE) cross peaks between SP and long-chain lipid molecules SP was probed to bind on the flat surface of the disc-like bicelles. Structural analysis of NMR data indicated that the helical conformation of SP extended to the C-terminal region of Leu10 as well as in the mid-region from Pro4 to Phe8. As compared with the conformations of SP bound on the sodium dodecylsulfate (SDS) or the dodecylphosphocholine (DPC) micelles with curved surfaces, the surface curvature of the membrane mimics was found to be one of the major factors inducing the biologically relevant conformation of SP. The negative surface charge of the membrane is also a key factor inducing both the binding of SP on the membrane and its biologically active structure.