• 한국동물위생학회지
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• 제22권1호
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• pp.15-23
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• 1999

A multiresidue, simple and rapid isolation technique known as matrix-solid phase dispersoin (MSPD) for the extraction and quantitative gas chromatographic/electron capture detection (GC/ECD) determination of 14 organochlorinated pesticides($\alpha$-BHC, ($\beta$-BHC, ($\gamma$-BHC, aldrin, dieldrin, endrin, heptachlor, ($\alpha$-endosulfan, ($\beta$-endosulfan, endosulfan sulfate, p,p'-DDE, o,p'-DDD, p,p'-DDD, p,p'-DDT) from meat fats. The 14 pesticide were fortified into meat fat(0.5g) and blend with 2g $C_{18}$, $C_{18}$meat fat matrix blend and 2g activated florisil comprise an extraction column from which the pesticides are eluted by adding 8ml acetonitrile. Then 2${\mu}\ell$ of the eluate is analyzed by GC/ECD. Unfortified blank controls are tested similarly. The eluate contained all the pesticide analytes and was free of interfering coextractants. Recovery rate(31.3-500ng/g) were ranged from 80$\pm$4% to 97$\pm$4%. Any organochlorinated pesticides were not detected in 120 samples of beef and pork collected from slaughter houses in Kyeonggi province.

• Bulletin of the Korean Chemical Society
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• 제29권2호
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• pp.352-356
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• 2008

An analytical method has been developed for measuring chlorostyrenes in fish tissue sample. Extraction of chlorostyrenes from fish tissue was carried out by ultrasonication using acetone/n-hexane (5:2, v/v) mixture. Most of the lipids in the extract were eliminated by freezing-lipid filtration, prior to solid-phase extraction (SPE) cleanup. During freezing-lipid filtration, about 90% of the lipids extracted from the fish samples were easily removed without any significant losses of chlorostyrenes. For purification, SPE using Florisil was used for the rapid and effective cleanup. Quantification was performed using gas chromatography-mass spectrometry in the selected ion monitoring mode. Spiking experiments were carried out to determine the recovery, precision, and limits of detection (LODs) of the method. The overall recovery was above 80% in the spiked fish tissue sample at 10 and 100 ng/g levels, respectively. The detection limits for chlorostyrenes were ranged from 0.05 to 0.1 ng/g. This developed method is demonstrated to give efficient recoveries and LODs for detecting chlorostyrenes spiked into fish tissue with high lipid content.

• 대한수의학회지
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• 제37권1호
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• pp.213-220
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• 1997

A simple and rapid method known as matrix solid phase dispersion(MSPD) for simultaneous determination of 11 pesticide(2,4,5,6-tetrachlor m-xylene, ${\alpha}$-BHC, ${\gamma}$-BHC, ${\delta}$-BHC, aldrin, chlorfulazuron, heptachloroepoxide, dieldrine, endrin, endosulfan sulfate, and tetradifon) in beef fat was estabilished. Beef fat(0.5g) was fortified by adding the 11 pesticides and dibutylchlorendate as internal standard, and blended with 2g bulk $C_{18}$ in pestle and motar. Pesticides were eluted from an extraction column composed of $C_{18}$/ fat matrix blend and 2g activated Florisil by addition of 8ml acetonitrile. Then $2{\mu}l$ portion of the acetonitrile elute was directly analyzed by gaschromatography with electron capture detection. Unfortified blank control were treated similarly. Recovery rate were ranged from $83{\pm}5.4%$ to $94.2{\pm}7.6%$, intra-assay variability and inter-assay variability were ranged from 2.3% to 7.4%(n=5 for each insecticides) and from $6{\pm}1%$ to $12{\pm}3%$(n=10 for each insecticides), respectively. These results indicated that the MSPD methodology is aceptable for the extraction, determination and screening of residues 11 chroniated pesticides in beef fat.

• Bulletin of the Korean Chemical Society
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• 제25권10호
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• pp.1489-1494
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• 2004

A gas chromatography/mass spectrometric assay method was developed for the determination of persistent organochlorine pollutants (POPs) in hair. For the exact extraction study was used hair of rat exposed with POPs. Sonication of the hair matrix with 3 M HCl solution in methylene chloride of the extraction methods studied was the most efficient and rapid sample preparation method. After sonication of rat hair was achieved clean up with a solid phase extraction procedure using silica gel-florisil. Elution was performed with 8 mL of methylene chloride. The eluate was concentrated to approximately 100 ${\mu}L$ and analyzed by gas chromatography-mass spectrometry (GC-MS). Detection limits of POPs were in the concentration range of 0.6-1.2 ng/g in rat hair. Aldrin, dieldrin, p,p-DDT and mirex were dosed rat for 4 weeks at concentration of 0.01 mg/L in drinking water and detected in rat hair at concentration of 2.8, 11.3, 7.9 and 15.6 ng/g, respectively. Aldrin and p,p-DDT were metabolized to dieldrin and p,p-DDE, which were detected in concentration of 9.7 and 2.9 ng/g in rat hair, respectively. The developed method may be valuable to be used to analyze POPs in human hair.

• Bulletin of the Korean Chemical Society
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• 제30권1호
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• pp.61-66
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• 2009

An analytical method based on solid-phase extraction and gas chromatography / mass spectrometry has been developed for measurement of acaricides (amitraz, bromopropylate, coumaphos, cymiazole, and tetradifon) in honey sample. In the stability test of acaricides in honey, amitraz underwent a rapid degradation into 2,4-dimethylaniline (DMA), 2,4-dimethylphenylformamide (DMPF), and N-(2,4-dimethylphenyl)-N'-methylformamidine (DMPMF), whileas other acaricides were found to be stable even for over three months. Extraction of five acaricides from 5g of honey sample was carried out by liquid-liquid extraction using 20mL of ethylacetate. For purification, Florisil-SPE cartridge with elution of 5mL of n-hexane/ acetone (55:45, v/v) was found to remove interferences effectively. Quantification was performed using gas chromatography / mass spectrometry in the selected ion monitoring mode. Spiking experiments were carried out to determine the recovery, precision, and limits of detection (LODs) of the method. The overall recovery values from honey spiked at 0.02 and 0.20 ${\mu}g/g$ levels, respectively, were found to be greater than 75% for all acaricides. The method detection limits for acaricides were ranged from 0.1 to 3 ppb. The developed method in this study was applied for the monitoring of acaricides in honey products collected from urban markets in Korea.

• Food Science and Biotechnology
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• 제16권1호
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• pp.150-153
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• 2007

Hydrocarbons have been successfully used as a chemical marker in order to identify irradiated from non-irradiated foods. The method for determining hydrocarbons consists of extraction of fats, followed by separation of hydrocarbons by florisil column chromatography, and then identification of hydrocarbons by GC/MS. Currently, solvent extraction method for fats has certain limitations with regard to extraction time and solvent consumption. Commercial hams and sausage were irradiated at 0 and 5 kGy, and the efficiency of microwave-assisted extraction (MAE) and conventional solvent extraction (CSE) methods on the extraction of radiation-induced hydrocarbons from the meat products was compared. Significant levels of hydrocarbons, mainly composed of 1,7-hexadecadien, 1,7,10-hexadecatriene, and 6,9-heptadecadiene, were detected in the extracts from irradiated hams and sausages by both CSE and MAE methods. Both methods were acceptable in extracting hydrocarbons from samples, but MAE method required apparently reduced amounts of solvent from 150 (CSE) to 50 mL and reduced extraction time from 23 (CSE) to 5 min.

• 한국환경농학회지
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• 제23권4호
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• pp.251-257
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• 2004

Analytical methods were developed to determine cyclosulfamuron residues in soil, water, rice grain and straw using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. In these methods, cyclosulfamuron was extracted with aqueous $Na_2HPO_4$/acetone and acetone/methanol mixture from soil and rice samples respectively. Liquid-liquid partition coupled with ion-associated technique, Florisil column chromatography, and solid-phase extraction (SPE) were used to separate cyclosulfamuron from interfering co-extractives prior to HPLC analysis. For water sample, the residue was enriched in $C_{18}$-SPE cartridge, cleaned up in situ, and directly subjected to HPLC. Reverse-phase HPLC under ion-suppression was successfully applied to determine cyclo-sulfamuron in sample extracts with the detection at its ${\lambda}_{max}$ (254 nm). Recoveries from fortified samples averaged $87.8{\pm}7.1%$ (n=12), $97.3{\pm}7.2%$ (n=12), $90.8{\pm}6.6%$ (n=6), and $78.5{\pm}6.7%$ (n=6) for soil, water, rice grain and straw, respectively. Detection limits of the methods were 0.004 mg/kg, 0.001 mg/L, 0.01 mg/kg and 0.02 mg/kg for soil, water, rice grain and straw samples, respectively.

• 한국환경농학회지
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• 제30권4호
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• pp.432-439
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• 2011

BACKGROUND: An official analytical method was developed to determine etofenprox residues in agricultural commodities using high-performance liquid chromatography (HPLC). METHODS AND RESULTS: The etofenprox residue was extracted with acetone from representative samples of five raw products which comprised rice grain, apple, mandarin, cabbage, and soybean. The extract was then serially purified by liquid-liquid partition and Florisil column chromatography. For rice and soybean samples, acetonitrile/n-hexane partition was additionally coupled to remove nonpolar lipids. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate etofenprox from co-extractives. Intact etofenprox was sensitively detected by ultraviolet absorption at 225 nm. Recovery experiment at the quantitation limit validated that the proposed method could apparently determine the etofenprox residue at 0.02 mg/kg. Mean recoveries from five crop samples fortified at three levels in triplicate were in the range of 93.6~106.4%. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types. A selected-ion monitoring LC/mass spectrometry with positive atmospheric-pressure chemical ionization was also provided to confirm the suspected residue. CONCLUSION(s): The proposed method is simple, rapid and sensitive enough to be employed in routine inspection or monitoring of agricultural products for the etofenprox residue.

• Toxicological Research
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• 제25권1호
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• pp.41-45
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• 2009

This study was conducted to monitor the level of bifenthrin residues in pear sprayed with 2% bifenthrin wettable powder (WP) at the recommended rate at four different schedules prior to harvest. The target analyte was extracted with acetone, partitioned into dichloromethane, and then purified by florisil chromatographic column. The residue determination was performed on a DB-5 capillary column using GC with electron capture detector (ECD). Linearity of this method was quite good ($r^2$ = 0.9951) in the concentration ranged from 0.2 mg/kg to 10 mg/kg. Recovery test was carried out at two concentration levels, 0.2 mg/kg and 1.0 mg/kg, in three replicates, and their rates were from 82.9% to 107.2%. No quantitative bifenthrin was detected in pear of all kinds of treatments including the treatment sprayed 4 times until 7 days before harvest. This sensitive and selective method can be used to monitor the trace residual amounts of bifenthrin in pear in a quite low concentration level.

• Preventive Nutrition and Food Science
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• 제9권3호
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• pp.222-226
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• 2004

Hydrocarbons induced by gamma-irradiation of green, black, and oolong teas were analyzed to determine whether the hydrocarbons can be used as markers for detecting post-irradiation of these teas. The samples were irradiated at 0, 2.5, 5, 7.5, and 10 kGy. Detection was attempted by extracting fat from the teas, separation of hydrocarbons with florisil column chromatography, and identification of hydrocarbons by gas chromatography-mass spectroscopy (GC-MS). Concentration of hydrocarbons increased with the irradiation dose. The major hydrocarbons in irradiated green, black, and oolong teas were 1-tetradecence (14:1), pentadecane (15:0), 1,7-hexadecadiene (16:2), 1-hexadecene (16:1), 8-heptadecene (17:1), and heptadecane (17:0). Radiation-induced hydrocarbons in teas were 1,7-hexadecadiene and 8-heptadecene. These compounds were not detected in non-irradiated samples, so the hydrocarbons (16:2, 17:1) can be used as markers for detecting post-irradiation of the teas. Furthermore, detection of hydrocarbons after 12 months storage at room temperature remains a suitable method for identifying irradiated teas.