• YAKHAK HOEJI
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• v.23 no.3_4
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• pp.187-189
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• 1979

A new method for the synthesis of azido and thiocyanatoindoles by iodine and sodium azide or sodium thiocyanate in acetonitile at room temperature or 60.deg.C was found. Azidoindoles (3-azido-3-methyl -2-phenylindolenine, 3-azido-2,3-diphenylindolenine, 2-azidomethyl-3-metbylindole and 1-azido-1,2,3,4-tetrahyrocarbazole) and thiocyanatoindoles(3-thiocyanatoindole, 2-phenyl-3-thiocyanato indole, 3-methyl-2-phenyl-6-thiocyanatoindole and 2, 3-diphenyl-6-thiocyanatoindole) were prepared by this method in good yields.

• Journal of the Korean Institute of Gas
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• v.13 no.2
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• pp.23-29
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• 2009

This study investigated sensitivity of the gas sensor to chemical weapons with the sensor material doped with catalysts. The nano-sized SnO2 powder mixed with metal oxides (TiO2) was doped with transition metals(Pt, Pd and In). Thick film of nano-sized SnO2 powder with TiO2 was prepared by screen-printing method onto Al2O3 substrates with platinum electrode and chemical precipitation method. The physical and chemical properties of sensor material were investigated by SEM/EDS, XRD and BET analyzers. The measured sensitivity to simulant toxic gas is defined as the percentage of resistance of value equation, [(Ra-Rg)/$Ra\;{\times}100$)], that of the resistance(Ra) of SnO2 film in air and the resistance(Rg) of SnO2 film in acetonitrile gas. The best sensitivity and selectivity of these thick film were shown with 1wt.% Pd and 1wt.% TiO2 for acetonitile gas at the operating temperature of $250^{\circ}C$.

• Analytical Science and Technology
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• v.16 no.1
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• pp.78-81
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• 2003

Peptides separation in high performance liquid chromatography (HPLC) is very important for the analysis of total proteins using mass spectrometry rather than two-dimensional polyacrylamide gel electrophoresis (2D-PAGE). In this study, we investigated the optimal HPLC condition of peptides for the use of mass fingerprinting. As a result of pursuing a combination of solvent additives for HPLC, water and acetonitile containing both 0.1% trifluoroacetic acid and 0.1% acetic acid respectively showed the most efficient resolution and sensitivity.

• Journal of the Korean Society of Tobacco Science
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• v.36 no.1
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• pp.12-19
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• 2014

A matrix solid-phase dispersion (MSPD) method was developed for extracting and cleaning-up the selected agrochemicals in tobacco using gas chromatography-mass spectrometry with selected ion monitoring (GC/MS-SIM). Different parameters of the method were investigated and optimized, such as the type of solid-phase (alumina, $C_{18}$ and Florisil) and eluent (acetone, acetonitrile, ethylacetate and n-hexane). The best results were obtained using 0.5 g of tobacco sample, 1.0 g of $C_{18}$ as dispersant sorbent, 1.0 g of Florisil as clean-up sorbent and acetonitile saturated with n-hexane as eluting solvent. The method was validated using tobacco samples fortified with agrochemicals at their different concentration levels. This method gave good linearity for the selected agrochemicals of ranging from $0.01{\mu}g/mL$ to $0.1{\mu}g/mL$. Recoveries of the selected agrochemicals in tobacco were more than 80 % and reproducibilities were found to be better than 10 % RSD. Those results suggested that the analytical procedure including MSPD method in combining with GC/MS could be applicable to the rapid determination often the selected agrochemicals in tobacco.

• Journal of Food Hygiene and Safety
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• v.8 no.1
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• pp.25-35
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• 1993

This study is conducted to deyelop more conyenient simultaneous determination method by HPLC for mixed antimicrobial agents (sulfamerazine; SMR, sulfamethazine; SMT, sulfamonomethoxine; SMMX, sulfadimethoxine; SDMX, sulfaquinoxaline; SQX, furazolidone; FZ, zolene; ZOL and ethopabate; EPB in muscles of boline, pork and chicken. The drugs were extracted by dichloromethane and water. The extract, after solyent eyaporation, was partitioned in hexane/water and water/dichloromethane. The dichloromethane layer was filtrated with anhydrous $Na_5S0_4\;in\;_3G_3$ glass filter and was eyaporated to dryness. The residue was dissoIYed in mobile phase. The test solution analyzed by HPLC. The chromatograpic conditions were as follows; Column-Spheri 5 RP-8($4.6{\times}220,\;5\;{\mu}$), Wayelength-270 nm, Mobile phase-acetonitrile: 0.005 M oxalic acid (22 : 78). The ayerage recoyeries of drugs from muscles of boline, pork and chicken spiked standard solution were approximately 74~99%, 73~99% and 75~96%, respectiyely. The limits of detection were 5 ppb for SMR, SMT, SMMX, SDMX and EPB, and 8 ppb for SQX, FZ and ZOL.

• Korean Journal of Environmental Agriculture
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• v.23 no.3
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• pp.158-169
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• 2004

For the improvement of gas chromatographic analysis of multiple pesticide residues in green pepper, lettuce and Chinese cabbage, multiresidue test mixtures (MRTMs) of 10 groups (ECD 5 groups and NPD 5 groups) and a recovery test mixture (RTM) of 18 compounds (11 compounds for ECD and 7 compounds for NPD) were established based on retention time and response to relevant detectors. A new extraction solvent (acetone: acetonitrile=1 : 9) and a clean up eluent (hexane: dichloromethane : acetonitile = 50 : 48.5 : 1.5) for solid-phase extraction (SPE) cartridge were selected to test two types of multiresidue methods (MRM I and MRM II). MRM II provided high recovery better than MRM I when RTM was tested Recovery experiment with MRTMs which was conducted using MRM II resulted in that more than seventy percents of compounds were recovered in the range of $50{\sim}140%$, while 9% of compounds were over 140% of recovery and only $7{\sim}8$ compounds failed to detect. MRM II, an improved method, could be employed for screening residues of 190 pesticides in those vegetables.

• Korean Journal of Pharmacognosy
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• v.44 no.1
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• pp.53-59
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• 2013

This study was conducted to determine the content of atractylenolides I and III in Atractylodes japonica. An established HPLC-DAD method was used to monitor contents of atractylenolides I and III in A. japonica obtained from Korea and China and compared with contents of A. macrocephala, A. chinensis, and A. lancea. Quantitative analysis of atractylenolides I and III was carried out on a Shiseido C18 column (S-5 ${\mu}m$, 4.6 mm I.D. ${\times}$ 250 mm) with gradient elution composed of acetonitile-water. The results show that the average content of atractylenolides I and III in A. japonica were 0.0954 and 0.1963%, respectively, and contents of A. lancea were higher than A. macrocephala, A. chinensis. In this study, we identified the differentiation of the quality of A. japonica from different species and collected locations and established content standard of atractylenolides I and III in A. japonica and this content standard was helpful to quality control of A. japonica.

• Journal of the Korean Chemical Society
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• v.37 no.6
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• pp.612-617
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• 1993

Some vanadium(III) complexes have been prepared from the reaction of VC$l_3$ with N, P, O-donating ligands and characterized by elemental analysis, $^1$H-NMR infrared and UV-Visible spectroscopy. 3,5-Lutidine, 1,2-phenylenediamine, 8-hydroxyquinoline, 9,10-phenanthrenequinone, triphenylphosphine, 1,2-bis(diphenylphosphino)ethane, 1,3-bis(diphenylphosphino)propane and 1,1'-bis(diphenylphosphino)ferrocene were chosen as coordinating ligands. Stretching frequency ${\nu}g$(V-Cl) of complexes appears) at 298∼367 cm-1, which show octahedral geometries. Stretching frequency of ${\nu}g$(V-X) (X = N, P, O) indicates that ligands are coordinated to vanadium(III). Stretching frequency ${\nu}g(C{\equiv}N)$ of acetonitrile in these complexes are characteristically shifted to about 70 c$m^{-1}$ higher compared with that of a free ligand (2260 c$m^{-1}$). Bending frequency of $\delta(C{\equiv}N)$ is also shifted to about 60 c$m^{-1}$ higher compared with that of a free ligand (377 c$m^{-1}$). Finally each vanadium(III) complex showed the following formulation; [VC$l_3$(L)$_2$MeCN] or [VC$l_3$(L-L)MeCN].

• Korean Journal of Weed Science
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• v.30 no.4
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• pp.361-370
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• 2010

This study was carried out to establish the analytical method of MCPA residue in brown rice and rice straw by HPLC/UVD. When MCPA was extracted from sample under the pH 3.6 by adding acetone 200 mL and 1N-HCl 100 mL, the extraction efficiency was high by 87%. And purification efficiency was high by 83% when 5 mL of 1% methanol/acetonitrile was eluated by the florisil Sep-pak cartridge column. From spiking of $0.1{\mu}g\;mL^{-1}$ and $0.25{\mu}g\;mL^{-1}$ of MCPA to control sample, respectively, average recovery rate of MCPA in brown rice was 96.0% and 94.9% and that in rice straw was 92.5% and 88.2%, respectively. Precision of experiment was very high by relative standard deviation of 1.5% to 5.7%. In brown rice and rice straw treated with bentazone+MCPA (11+1.2%) of 30 kg and 60 kg per ha at 30 days after rice transplanting, respectively, maximum residue limit was under $0.05{\mu}g\;mL^{-1}$ of the recommended rate of Korean Food and Drug Administration. From the above results, the analytical procedure of MCPA in plants such as hydrolysis, saponification and derivatization were ommited, and retention time was faster and recovery rate was higher than the existed results of HPLC/UVD. Therefore, these results were greatly improved and seemed to be usefully applied for residue analysis of MCPA in plants.

• Korean Journal of Environmental Agriculture
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• v.26 no.3
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• pp.246-253
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• 2007

This study was performed to enhance the cleanup efficiency of methoxyfenozide and bentazone by pH adjustment in the course of liquid-liquid partition and to develop an optimum analytical conditions using HPLC coupled with DAD for two matrices, brown rice and rice straw. Preparation procedure of brown rice sample was "extraction${\rightarrow}$coagulation${\rightarrow}$liquid-liquid partition$\rightarrow$-florisil C.C", and this procedure was samely applied to two compounds. In rice straw, preparation procedure of methoxyfenozide sample was "extraction$\rightarrow$-alkalization$\rightarrow$liquid-liquid extraction$\rightarrow$coagulation$\rightarrow$florisil C.C", and in the case of bentazone, "extraction$\rightarrow$alkalization$\rightarrow$liquid-liquid partition$\rightarrow$acidification$\rightarrow$liquid-liquid extraction$\rightarrow$florisil C.C". All these purified samples were redissolved in the mobile phases, acetonitile : 20 mM sodium acetate (75:25, v/v) for methoxyfenozide and acetonitrile : 75 mM sodium acetate, pH 6.0 (40:60, v/v) for bentazone. Recoveries of methoxyfenozide analysis in brown rice and rice straw were 83.5-97.4 and 86.4-97.3%, and detection limits were 0.02 and 0.04 mg/kg, respectively. Recoveries of bentazone in brown rice and rice straw were 86.8-101.9 and 88.3-94.5% and detection limits were 0.005 and 0.01 mg/kg, respectively. This methods seem to be usefully applied to the residue analysis of two compounds in the view of producing stable analytical condition and fair reproducibility.