• Proceedings of the Korean Society of Crop Science Conference
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• 1997.05a
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• pp.112-113
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• 1997

• Bulletin of the Korean Chemical Society
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• v.16 no.5
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• pp.422-427
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• 1995

In a stream of water sample, trace metal ions are quantitatively coprecipitated with Indium hydroxide and filtered. The filtered precipitate is continuously dissolved in 3 M nitric acid and introduced to ICP directly. The lead, cadmium, and copper are concentrated more than 10-fold and determined with ICP-AES at a sampling frequency of 10/hour. The detection limits are 2.89, 1.43,0.52 ppb for lead, cadmium, and copper respectively. Recoveries of lead, cadmium, and copper are 98.7, 94.3, and 104.5% respectively. The RSD values for three elements are about 3-5% currently.

• Bulletin of the Korean Chemical Society
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• v.19 no.12
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• pp.1351-1355
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• 1998

A simple apparatus for adding a modifying solvent to supercritical CO2 extractant was described. Small, fixed volumes (typically 100 μL) of liquid modifying solvents were delivered during the extraction process by use of an in-line high pressure loop injector and an air pump. Without disconnecting the extraction cell from the supercritical fluid extraction system, the modifying solvent was repeatedly delivered. The solvent modification device was optimized during the extraction of carbaryl and bis(acetylacetonato) copper(Ⅱ). Extraction recoveries from spiked filter paper and soil samples ranged between 22% and 109%, depending on the analyte and matrix components. The addition of polar modifying solvents were necessary to improve the extractability of the nonpolar CO2.

• Korean Journal of Environmental Agriculture
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• v.34 no.2
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• pp.128-133
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• 2015

BACKGROUND: Plant extracts have been used as environment friendly agricultural materials for organic farming in South Korea. However safety evaluation on the plant extracts was not properly tested. The aim of this study was to evaluate safety of the extracts from Melia azedarach, Nerium indicum and Coptis chinensis on cultivating rice. METHODS AND RESULTS: Pant extarcts 300-fold diluted were treated on rice, and residues of M. azedarach, N. indicum and C. chinensis were determined. The analytes from the rice samples were detected by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). The method was validated, and good linearities ($r^2=0.995-0.998$), specificity, and recoveries were obtained. Limits of detection were 0.01 mg/kg for all of the target compounds. Recoveries were 79.3-118.3% at 0.1 mg/kg and 75.2-111.5% at 0.5 mg/kg. The residue levels were below 0.030 mg/kg for azadirachtin, 0.320 mg/kg for oleandrin and 1.460 mg/kg for berberine. CONCLUSION(S): The extracts of M. azedarach, N. indicum and C. chinensis contained azadirachtin, oleandrin and berberine as an active ingredient, respectively. The residue of three active ingredients dramatically decreased after treatment in all fruits, stems and roots of rice.

• Bulletin of the Korean Chemical Society
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• v.27 no.9
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• pp.1293-1296
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• 2006

In this study, a solid phase extraction method has been developed for the preconcentration and separation of the elements Cr(III), Fe(III), Co(II) and Pb(II) at trace levels by using a column packed with Amberlite XAD-1180 resin loaded with 4-(2-pyridylazo)-resorcinol (PAR) reagent. After preconcentrating, the metals retained on the column were eluted with 20 mL of 3 mol/L $HNO_3$ and then determined by flame atomic absorption spectrometry (FAAS). The factors affecting the recovery of the elements, such as pH, type and concentration of eluent, volume of sample and elution solution, and matrix components, were also ascertained. The recoveries of Cr(III), Fe(III), Co(II) and Pb(II) were found to be $99\;{\pm}\;4,\;97\;{\pm}\;3,\;95\;{\pm}\;3$ and $98\;{\pm}\;4$%, respectively, under the optimum conditions at 95% confidence level and the relative standard deviations found by analyzing of nine replicates were $\leq4.4$%. The preconcentration factors for Cr(III), Fe(III), Co(II) and Pb(II) were found as 75, 125, 50 and 75 respectively. The detection limits (DL, 3s/b) were 3.0 $\mu g/L$ for Cr(III), 1.25 $\mu g/L$ for Fe(III), 3.3 $\mu g/L$ for Co(II), and 7.2 $\mu g/L$ for Pb(II). The recoveries achieved by adding of metals at known concentrations to samples and the analysis results of Buffalo river sediment (RM 8704) show that the described method has a good accuracy. The proposed method was applied to tap water, stream water, salt and street dust samples.

• Bulletin of the Korean Chemical Society
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• v.24 no.4
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• pp.413-420
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• 2003

A gas chromatography/mass spectrometric assay method was developed for the simultaneous determination of neutral and bacis twenty-five disruptors $(ED_S)$ in frog and fish. Afther homogenization and sonication of 5 g of sample, purification was achieves in one step with a solid phase extraction procedure using silica gelflorisl. Eluton was performed with 50mL of acetone : n-hexane (1 : 9) solution. The eluate was concentrated to approximately 10uL and dissolves with 100 uL of hexane and analyzed by GC-MS (SIM). The peaks had good chromatographic properties and the extraction of these compounds from sample also gave relatively high recoveries with small variatoins. Detection limits were 0.1 ng/g for 4-nitrotoluene, benzophenone, hexachlorobenzene, atrazine, malathion, o,p-DDT, o,p-DDT and permethrin, and 0.2 ng/g for heptachlor epoxide, γ-chlordane, α-chlordane, p,p'-DDE, p,p'-DDD, cypermethrin and fenvalerate, and 0.3 ng/g for trifluralin, metribuzin, alachlor, dieldrin and p,p'-DDT, and 0.5 ng/g for heptachlor, aldrin and parathion, and 0.7 ng/g for endrin, and 0.8 ng/g for nitrofen. The recoveries were between 33 and 109%. The method was used to analyze twenty-five frogs and forty-six fishes fishes samples caught from various regions in Korea. Benzophenone was detected at concentration of up to 17.2 ng/g in frog or fish. Heptachlor, aldrin, γ-chlordane, p,p'-DDE, p,p'-DDD, endrin and o,p-DDD were detected at concentrations of 0.7-12.5 ng/g in frog or fish. Also significant leveles of dieldrin (up to 22.5 ng/g) were observed. The developed method may be valuable to be used to the national monitoring project of EDS in biota samples.

• Analytical Science and Technology
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• v.14 no.2
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• pp.95-102
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• 2001

A comprehensive analytical method of endocrine disruptors[i.e., nonylphenol(NP), octylphenol(OP), bis(2-ethylhexyl) phthalate(BEHP)] in meat or pork samples was developed. The method employed closed culture tube extraction with dichloromethane and solvent exchange to iso-hexane and SPE(2g) aminopropyl column, followed by determination on gas chromatography linked to mass spectrometry(GC/MS) operated in the single ion monitering(SIM) mode. For the multipoint recovery of nonylphenol, octylphenol and bis(2-ethlhexyl) phthalate OP, NP were showen good recoveries in $0.125-1.25{\mu}g/g$ range of concentration, and BEHP more good recoveries in $0.0125-12.5{\mu}g/g$ wide range of concentration. The present method was applied to beef or pork samples of mart and butcher in Cheonju city and near Cheonju. The range of concentrations was respectively, $0.06-0.24{\mu}g/g$ in nonylphenol(NP) and $0.36-2.35{\mu}g/g$ in bis(2-ethylhexyl) phthalate(BEHP), but octylphenol(OP) was not dected in any samples. This method provides a powerful analytical tool to investigate a wide range of endocrine disruptors in biological samples of limited quantity.

• Korean Journal of Environmental Agriculture
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• v.32 no.2
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• pp.136-141
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• 2013

BACKGROUND: This study was performed to establishment the PHRLs of peach during cultivation period, and also to estimate biological half-lives for residues of fenarimol and flufenoxuron. METHODS AND RESULTS: The extracted samples of fenarimol were analyzed by GC-ECD and the flufenoxuron extracted samples were analyzed by HPLC-DAD. Recoveries of fenarimol at two fortification levels of 0.1 mg/kg, 0.5 mg/kg were $93.69{\pm}6.56$(%) and $94.45{\pm}1.60$ (%), respectively. And recoveries of flufenoxuron at two fortification levels of 0.1 mg/kg, 0.5 mg/kg were $106.73{\pm}5.90$(%) and $96.37{\pm}6.66$(%), respectively. CONCLUSION(S): The biological half-lives of fenarimol in single treatment and triple treatment were 3.5day and 3.8day. that of Flufenoxuron was also 7.1day and 4.9day, respectively. The PHRL of fenarimol were recommended as 1.5 mg/kg for 10day before harvest and the PHRL of flufenoxuron were recommended as 1.4 mg/kg for 10day before harvest.

• Analytical Science and Technology
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• v.9 no.2
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• pp.123-133
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• 1996

The optimum conditions for the analysis of the difenoconazole fungicide on soil and crops were investigated and the residues of that in apple and soil were identified by using the gas chromatography. The extract with acetonitrile was separated with saturated NaCl and n-hexane solution after filtered, and concentrated. Obtained fungicide residues were transfered to the florisil column and eluted with acetone and n-hexane mixed solution for the analysis by GLC(ECD). From the standard addition experiments with 0.20 and 1.0ppm, the average recoveries were 86~92% and the detection limit was 0.01 ppm. It seems to be safely used when difenoconazole is treated three times until 15 days before harvest of apple. In this case residual amounts of difenoconazole in apple was from 0.037ppm to 0.044ppm. The soil samples extracted with methanol and ammonium hydroxide mixed solution were partitioned with dichloromethane and saturated sodium chloride solution. The organic phase was concentrated and redissolved with toluene and analyzed with GLC(FID) after cleaned with Sep-Pak column. From the standard addition experiments with 0.10, 0.50 and 1.0ppm, the average recoveries were 101.2~103.7% and the detection limit was 0.025ppm.

• Bulletin of the Korean Chemical Society
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• v.28 no.3
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• pp.432-438
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• 2007

Environmentally important phthalic esters have been analyzed by GC-MS in terms of individual phthalic esters or total phthalic esters directly or after derivatization. Derivatization improves the chromatographic characteristics of the highly polar phthalic esters. This study focused on the GC-MS determination of the total phthalic esters and the individual phthalic esters simultaneously. The phthalic esters were hydrolyzed to phthalate and corresponding alcohols in 1 M NaOH solution at 90 oC for 30 min followed by extraction with ethyl acetate after acidifcation. The phthalic acid and alcohols were simultaneously silyl derivatized using bis(trimethylsilyl)trifluoroacetamide (BSTFA) to their corresponding silyl ester and ethers in the mixture of 60% acetone and 40% ethyl acetate at room temperature within 30 min. Because of the high reactivity of BSTFA with the phthalic acid and alcohols effective silyl derivatization was possible simultaneously. GC-MS analysis of the silyl derivatives of phthalic acid and alcohols was performed. The total phthalic ester content was estimated from the analytical result of phthalic silyl ester, while the individual phthalic ester was quantified from the analytical results of alcoholic silyl ethers. This technique was applied to spiked tab water and real seawater samples from the Lake Shihwa in Korea. The results were checked against the results from the direct GC-MS analysis of the phthalic esters and reasonable recoveries with high sensitivity were achieved. The recoveries were higher than 75% with low relative standard deviation (below 10%).