• Bulletin of the Korean Chemical Society
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• v.27 no.9
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• pp.1315-1322
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• 2006

The following study describes the gas chromatography-mass spectrometry (GC-MS) based screening and confirmation analysis of urinary androgenic steroids. Four commercially available solid-phase extraction (SPE) cartridges, Serdolit PAD-1, Sep-pak $C_{18}$, amino-propyl, and Oasis HLB, and three different extractive organic solvents, diethyl ether, methyl tert-butyl ether (MTBE), and n-pentane, were tested for sample preparation. Overall, Oasis HLB combined with MTBE extraction provided the highest recoveries in 39 of 46 total androgenic steroids examined and it showed a good extraction yield (>82.1%) for polar steroids, such as metabolites of fluoxymesterone, oxandrolone, and stanozolol, which gave a poor recovery in both n-pentane (9.2-64.3%) and diethyl ether (22.2-73.6%) extractions. All SPE sorbents tested showed potential, because they were efficient in extraction for most or selective steroids. When applied to positive urine samples based on the results obtained, the present method allowed selective and sensitive analysis for detection of urinary androgenic steroids. The experiments showed that the high-resolution MS method is clearly more efficient than the low-resolution MS technique for the detection of many urinary steroids. However, comprehensive sample clean-up procedures also might be needed especially in confirmation analysis to increase detectability.

• Bulletin of the Korean Chemical Society
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• v.35 no.5
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• pp.1440-1448
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• 2014

Co(II)-tetrasulfonated phthalocyanine (CoTSP) is known to be aggregated to dimer at high concentration levels in water. A study on the aggregation of CoTSP using multivariate curve resolution analysis of the visible absorbance spectra over a concentration range of 30, 40 and 50 ${\mu}M$ in the presence of dimethyl sulfoxide (DMSO), dimethyl formamide (DMF), acetonitrile (AN) and ethanol (EtOH) in the concentration range of 0 to 3.57 M is conducted. A hard modeling-based multivariate curve resolution method was applied to determine the dissociation constants of the CoTSP aggregates at various temperatures ranging from 25, 45 and $65^{\circ}C$ and in the presence of various co-solvents. Dissociation constant for aggregation was increased and then decrease by temperature and concentration of phthalocyanine, respectively. Utilizing the vant Hoff relation, the enthalpy and entropy of the dissociation equilibriums were calculated. For the dissociation of both aggregates, the enthalpy and entropy changes were positive and negative, respectively. Molecular dynamics simulation of cosolvent effect on CoTSP aggregation was done to confirm spectroscopy results. Results of radial distribution function (RDF), root mean square deviation (RMSD) and distance curves confirmed more effect of polar solvent to decrease monomer formation.

• Analytical Science and Technology
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• v.30 no.3
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• pp.138-145
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• 2017

Microwave-assisted organic synthesis has gained a remarkable interest over the past years because of its advantages - (i) rapid energy transfer and superheating, (ii) higher yield and rapid reaction, (iii) cleaner reactions. Ionic liquids are well known for their unique properties such as negligible vapor pressure and high thermal stability. With these properties, ionic liquids have gained increasing attention as green, multi-use reaction media. Recently, ionic liquids have been applied as reaction media for biocatalysis. Lipase-catalyzed reactions in ionic liquids provide high activity and yield compared to conventional organic solvents or solvent free system. Since polar molecules are generally good absorbent to microwave radiation, ionic liquids were investigated as reaction media to improve activity and productivity. In this study, therefore, the effect of microwave irradiation in ionic liquids was investigated on lipase catalyzed reactions such as benzyl acetate synthesis and caffeic acid phenethyl ester synthesis. Comparing to conventional heating, microwave heating showed almost the same final conversion but increased initial reaction rate (3.03 mM/min) compared to 2.11 mM/min in conventional heating at $50^{\circ}C$.

• Journal of Marine Bioscience and Biotechnology
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• v.11 no.2
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• pp.36-41
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• 2019

This study was conducted to analyze the difference in mechanically improved properties by distinguishing α-chitin and β-chitin for Poly(L-lactic acid)(PLLA). First, dissolution of chitins was established by mixing polar solvents hexafluoroisopropanol (HFIP) and trifluoroacetic acid (TFA) in appropriate proportions. Under these conditions, the dissolved chitin was used for electrospinning with other polymers. The electrospun nanofibers of the PLLA and chitins were successfully produced. Compared to the pristine state, when chitin was added to PLLA, the tensile strength increased 1.41 times (α-chitin), by 1.61 times (β- chitin), respectively. Based on this, it was confirmed that α- and β- chitin could be strategically used for different polymers. The results also suggest that chitin can be applied to various fields as good reinforcing material as well as electrospinning.

• Microbiology and Biotechnology Letters
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• v.28 no.1
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• pp.26-32
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• 2000

Electrostatic forces contribute to the high degree of enzyme transition state complementarity in enzyme catalyzed reaction and such forces are modified by the solvent through its dielectric constant and polar properties. The contributions of electrostatic interaction to the formation of ES complex and the stabilization of transition state of the trypsin catalyzed reaction were probed by kinetic studied with high pressure and solvent dielectric constant. A good correlation has been observed between the increase of catalytic efficiency of trypsin and the decrease of solvent dielectric constant. Activation volume linearly decreased as the dielectric constant of solvent decreased, which means the increase in the reaction rae. Moreover, the decrease of activation volume by lowering the solvent dielectric constant implies a solvent penetration of the active with and a reduction of electrostatic energy for the formation of dipole of the active site oxyanion hole. When the 야electric constant of the solvents was lowered to 4.7 unit, the loss of activation energy and that of free energy of activation were 2.262 KJ/mol and 3.169 KJ/mol, respectively. The results of this study indicate that the high pressure kinetics combined with solvent effects can provide unique information on enzyme reaction mechanisms, and the controlling the solvent dielectric constant can stabilize the transition state of the trypsin-catalyzed reaction.

• Analytical Science and Technology
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• v.11 no.5
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• pp.341-346
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• 1998

2-Pyridinecarboxaldehyde thiocarbohydrazone(PyTC) have been reacted with $Cu^{2+}$ to form $[Cu(PyTC)H_2O)]SO_4$. This complex is soluble in water and polar organic solvents. The complex has been characterized by elemental analysis, conductivity, effective magnetic moment, and spectroscopic data. From the results the complex is square planar. The colorimetric determination of Cu(II) ion by using PyTC as a ligand was studied. The solution of copper(II) with PyTC was obeyed Beer's law in concentration up to $2.9{\times}10^{-4}M$ at pH 4.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.11 no.6
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• pp.2311-2316
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• 2010

Three series of copolyterephthalamides having biphenyl-2,2'-diyl structure in the main chain, were synthesized from p-phenylene-containing diamines such as p-phenylene diamine, 4,4'-oxydianiline or 1,4-bis(4-aminophenoxy)benzene, with mixed diacids of terephthalic acid and 2,2'-bibenzoic acid by the direct polycondensation method. The resulting copolymers had inherent viscosities ranging from 0.46 to 0.93dL/g, and most of them could be readily dissolved in polar aprotic solvents including N,N-dimethyl acetamide and N-methyl-2-pyrrolidone. These copolymers had glass transition temperatures between 239 and $326^{\circ}C$, and their 10% weight loss temperatures were recorded in the range of $410{\sim}485^{\circ}C$ in nitrogen atmosphere.

• ETRI Journal
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• v.27 no.2
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• pp.181-187
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• 2005

Alkoxy-substituted poly(spirobifluorene)s and their copolymers with a triphenylamine derivative have been synthesized by Ni(0)-mediated polymerization. The polymers were well soluble in common organic solvents. Pure blue-light emissions without the long wavelength emission of poly(fluorene)s have been observed in the fluorescence spectra of polymer thin films. The light emitting diodes with a device configuration of ITO/PEDT:PSS(30 nm)/polymer(60 nm)/LiF(1 nm)/Al(100 nm) have been fabricated. The electroluminescence spectra showed the blue emissions without the long wavelength emission as observed in the fluorescence spectra. The relatively poor electroluminescence quantum yield of the homopolymer (0.017% @ 20 $mA/cm^{2}$) with color coordinates of (0.16, 0.07) has been improved by the introduction of triphenylamine moiety, and the copolymer with derivative exhibited an electroluminescence quantum yield of 0.15 % at 20 $mA/cm^{2}$ with color coordinates of (0.16, 0.08). Moreover, the introduction of polar side chains to the spirobifluorene moiety enhanced the device performance and led to the quantum yields of 0.6 to 0.7 % at 20 $mA/cm^{2}$, although there was some expense of color purities.

• Macromolecular Research
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• v.14 no.4
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• pp.438-442
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• 2006

Novel sulfonated poly(aryl ether ketones) containing benzoxazole were directly synthesized by aromatic nucleophilic polycondensation using various ratios of 2,2'-bi[2-( 4-flurophenyl)benzoxazol-6-yl]hexafluoropropane to sodium 5,5'-carbonylbis(2-fluorobenzenesulfonate). The copolymers were soluble in polar aprotic solvents such as N-methyl-2-pyrrolidone, N,N-dimethylacetamide, and N,N-dimethylformamide at a relatively high solid composition (>15 wt%) and formed tough, flexible and transparent membranes. The membranes exhibited a degradation temperature of above $290^{\circ}C$. The exact dissolution times of these membranes at $80^{\circ}C$ in Fenton's reagent (3 wt% $H_2O_2$ containing 2 ppm $FeSO_4$) were undetectable, confirming their excellent chemical stability in fuel cell application. The membranes showed a moderate increase in water uptake with respect to increasing temperature. The proton conductivities of the membranes were dependent on the composition and ranged from $1.10{\times}10^{-2}$ to $5.50{\times}10^{-2}Scm^{-1}$ at $80^{\circ}C$ and 95% relative humidity (RH). At $120^{\circ}C$ without externally humidified conditions, the conductivities increased above $10^{-2}Scm^{-1}$ with respect to increasing benzoxazole content, which suggested that the benzoxazole moieties contributed to the proton conduction.

• Journal of the Korean Chemical Society
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• v.33 no.5
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• pp.530-537
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• 1989

Diethylbenzoylmalonates with various substituents were synthesized in moderately good yields through palladium-catalyzed carbonylative coupling of aryl iodide and diethylmalonate with carbon monoxide. Palladium-catalyzed carbonylative coupling reaction usually proceeded well in polar aprotic solvents in the presence of three equivalents of inorganic bases and palladium(II) catalyst. When the reaction was carried out under 10 atm pressure of carbon monoxide, the yield of diethylbenzoylmalonate derivatives was much better than that of reaction under atomspheric pressure of carbon monoxide.