• Korean Journal of Food Science and Technology
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• v.45 no.1
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• pp.20-24
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• 2013

Food irradiation has recently become one of the most successful techniques to preserve food with increased shelf life. This study aims to analyze hydrocarbons in almonds (Prunus amygosalus L.) and peanuts (Arachis hypogaea) induced by electron beam irradiation. The samples were irradiated at 0, 1, 3, 5 and 10 kGy by e-beam and using florisil column chromatography fat, and content was extracted. The induced hydrocarbons were identified using gas chromatography-mass spectrometry (GC/MS). The major hydrocarbons in both irradiated samples were 1,7-hexadecadiene ($C_{16:2}$) and 8-heptadecene ($C_{17:1}$) from oleic acid, 1,7,10-hexadecatriene ($C_{16:3}$) and 6,9-heptadecadiene ($C_{17:2}$) from linoleic acid and 1-tetradecene ($C_{14:1}$) and pentadecane ($C_{15:0}$) from palmitic acid. Concentrations of the hydrocarbons produced by e-beam were found to be depended upon the composition of fatty acid in both almonds and peanuts. The $C_{n-2}$ compound was found to be higher than $C_{n-1}$ compound in oleic acid and palmitic acid, while in case of linoleic acid, $C_{n-1}$compound was higher than $C_{n-2}$ compound. The radiation induced hydrocarbons were detected only in irradiated samples, with 1 kGy or above, and not in the non-irradiated ones. The production of 1,7-hexadecadiene ($C_{16:2}$), 8-heptadecene ($C_{17:1}$), 1,7,10-hexadecatriene ($C_{16:3}$) and 6,9-heptadecadiene ($C_{17:2}$), in high concentration gave enough information to suggest that these may be the possible marker compounds of electron beam irradiation in almonds and peanuts.

• Journal of Environmental Science International
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• v.15 no.1
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• pp.85-94
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• 2006

The simultaneous analysis of multi-residual pesticides was developed using a gas chromatography (GC) method. In this study, a simple and reliable methodology was improved to detect 154 kinds of pesticides in sinseng extract sample by using a liquid-liquid extraction procedure, open column chromagraphy and chromatographic analysis by CC electron capture detector (ECD) and GC nitrogen-phosphorus detector (NPD). The 154 kinds of pesticides were classified in 4 groups according to the chemical structure. The extraction of pesticides was experimented with $70\%$ acetone and dichloromethane/petroleum ether in order, and cleaned up via open column chromatography $(3\times30cm)$ packed with florisil $(30g,\;130^{\circ}C,\;12hrs)$. The final extract was concentrated in a rotator evaporator at $40^{\circ}C$ until dryness. Then the residue was redissolved to 2ml with acetone, and analyzed by GC-ECD and GC-NPD. The applied concentration of pesticides was over $1\~10{\mu}g/ml$. The recovery tests were ranged from $70.7\%$ to $115.2\%$ with standard deviations between 0.3 and $5.7\%$ of the standard spiked to the ginseng extract sample (Group $I\~IV$). The limit of detection (LOD) ranged from 0.001 to $0.099{\mu}g/ml$ (Group $I\~IV$). The 9 kinds of pesticides were not detected. The developed method was applied satisfactory to the determination of the 154 kinds of pesticides in the ginseng extract with good reproducibility and accuracy.

• Journal of the Korean Society of Food Science and Nutrition
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• v.43 no.12
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• pp.1889-1895
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• 2014

Radiation-induced hydrocarbon contents of dried anchovy, jiri anchovy, and large-eyed herring were evaluated following electron-beam irradiation at doses of 1, 3, 5, 7, and 10 kGy. GC/MS identification of the induced hydrocarbons by irradiation was conducted after lipid separation by soxtec, followed by florosil column chromatography. 1-Tetradecene ($C_{14:1}$) and pentadecane ($C_{15:0}$) derived from palmitic acid, 1-hexadecene ($C_{16:1}$) and heptadecane ($C_{17:0}$) from stearic acid, and 8-heptadecene ($C_{17:1}$) and 1,7-hexadecadiene ($C_{16:2}$) from oleic acid were the major induced hydrocarbons in irradiated dried anchovy, jiri anchovy, and large-eyed herring samples. At the same irradiation dose, concentration of induced hydrocarbons differed from fatty acid composition and increased in accordance with radiation dose level. Radiation-induced hydrocarbons, such as 1-tetradecene ($C_{14:1}$), 1-hexadecene ($C_{16:2}$), 8-heptadecene ($C_{17:1}$), and 1,7-hexadecadiene ($C_{16:2}$), were confirmed as irradiation marker compounds. Therefore, these marker compounds could be used to distinguish electron-beam irradiated dried anchovy, jiri anchovy, and large-eyed herring from non-irradiated ones.

• Korean Journal of Food Science and Technology
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• v.45 no.3
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• pp.285-292
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• 2013

This study was carried out to validate the safety of ametoctradin residues in agricultural commodities by developing an official analysis method. An analytical method was developed and validated using HPLC-PDA detectors. The samples were extracted with methanol, subsequently partitioned with dichloromethane and purified with florisil column chromatograph using acetone/hexane (30/70, v/v) as solvent. The method was validated by using grape, hulled rice, mandarin, and potato spiked with ametoctradin at 0.05 and 5.0 mg/kg, and pepper at 0.05 and 2.0 mg/kg. Average recoveries were 76-114.8% with relative standard deviation less than 10%, and the limit of detection and limit of quantification were 0.0125 and 0.05 mg/kg, respectively. The result of recoveries and overall coefficient of variation of the laboratory results from Gwangju regional Food and Drug Administration (FDA) and Daejeon regional FDA was accorded with Codex Alimentarius Commission Guideline (CAC/GL 40). Based on these results, this method was found to be appropriate for ametoctradin residue determination and can be used as the official method of analysis.

• Journal of the Korean Society of Food Science and Nutrition
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• v.33 no.9
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• pp.1522-1528
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• 2004

Electron spin resonance (ESR) and hydrocarbon characteristics were analyzed to establish identification conditions for irradiated dried red pepper. The ESR spectroscopy for 4 different parts (powder, pericarp, seed, stem) of the samples showed that irradiated samples signaled (g=2.024, 2.006, 1.987) a pair of peaks from a cellulose radical at intervals of 6 mT, which were not found on the non-irradiated samples. The ESR signals increased in directly proportion to the irradiation doses, which were still detectable after 12 weeks of storage at room temperature. The GC-MS analysis of hydrocarbons after fat extraction and separation by florisil column chromatography revealed that hydrocarbons, such as 1-tetradecene (14:1), 1,7,10-hexadecatriene (16:3), 1,7-hexadecadiene (16:2), 1-hexadecene (16:1), 6,9-heptadecadiene (17:2), and 8-heptadecene (17:1), were detected only from the irradiated samples immediately after irradiation and 8 months of storage. They linearly increased with the dose of irradiation, suggesting them as radiation-induced markers for irradiated dried red pepper.

• Toxicological Research
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• v.24 no.1
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• pp.87-91
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• 2008

The present study was conducted to monitor the level of triflumizole residues in fruits (apple and pear) and vegetable (cucumber) samples in order to assess risk posed by the presence of such residues to the consumer. Triflumizole was applied at a recommended dose rate to apple and pear pulps and to a cucumber sample. The samples were collected at harvesting time following several treatments (three and/or four treatments). Triflumizole was extracted with methanol and re-extracted into dichloromethane. The presence of triflumizole was determined by HPLC with UV detection at 238 nm following the cleanup of the extract by open preparative chromatographic column with Florisil. The versatility of this method was evidenced by its excellent linearity (> 0.999) in the concentration range between 0.2 and 4.0 mg/kg. The mean recoveries evaluated from the untreated samples spiked at two different fortification levels. 0.1 and 0.4 mg/kg, and ranged from 87.5${\pm}$0.0 to 93.3${\pm}$2.6 for the tested fruits and vegetable, respectively, and the repeatability (as relative standard deviation) from three repetitive determinations of recoveries were no larger than 6%. The calculated limit of detection was 0.02 mg/kg and the minimum detectable level of 4 ng for triflumizole was easily detected. When triflumizole was sprayed onto the apple trees three times at 50-40-30 and 40-30-21 days prior to harvesting and four times onto the pear trees at 40-30-21-14 days prior to harvesting, the mean residual amounts of 0.05 and 0.06 mg/kg for apples and pears, respectively, were not detected in all of the treatments. When the cucumber sample was fumigated four times at 7, 5, 3 and 1 day prior to harvesting, the mean residual amount was not detectable. Triflumizole can be used safely when sprayed (wettable powder, 30% active ingredient) and fumigated (10%) 4 times at 14 and 1 day prior to harvesting to protect the fruits and vegetable, respectively.

• Korean Journal of Environmental Agriculture
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• v.28 no.3
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• pp.281-288
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• 2009

The strobilurin fungicides, azoxystrobin and kresoxim-methyl, were investigated to know the biological half-lives and dissipation patterns in Korean melon under plastic film house condition. Used pesticides for field application were 20% azoxystrobin of suspension concentrate and 47% kresoxim-methyl of water dispersible granule. Two pesticides were sprayed at recommended and double dose rate. Pesticide residues in Korean melon were analyzed until 14 days after application. The azoxystrobin was analyzed by HPLC equipped with UV detector after cleanup with florisil glass column. Initial residue concentrations of azoxystrobin in Korean melon at recommended and double dose rate were 0.09 mg/kg and 0.14 mg/kg, respectively. Those were less than 0.2 mg/kg maximum residue limit of Korean melon established by KFDA. The biological half-lives of azoxystrobin in Korean melon were 4.7 days at recommended dose rate and 7.8 days at double dose rate. Initial concentrations of kresoxim-methyl which was analyzed by GLC-ECD in Korean melon at recommended and double dose rate were 0.10 mg/kg and 0.23 mg/kg, respectively. Those were less than 1.0 mg/kg, MRL. The biological half-lives of kresoxim-methyl in Korean melon were 4.1 days at recommended dose rate and 4.8 days at double dose rate. The residue amounts of both pesticide was lower than MRL and biological half-lives were not so long. Because the weight of Korean melon under plastic film house condition was fast increased during cultivation.

• Korean Journal of Environmental Agriculture
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• v.31 no.2
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• pp.146-151
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• 2012

BACKGROUND: This study was conducted to develop analytical method for picoxystrobin in agricultural commodities using GC/ECD and GC/MS. METHODS AND RESULTS: Each steps of analytical method were optimized for determining picoxystrobin residues in various agricultural commodities. The developed methods include acetone extraction, n-hexane/saline water partition and florisil column chromatography for analysis of all samples (apple, potato, green pepper, hulled rice and soybean), and in addition to these steps, solid phase extraction (SPE) was used for analysis of green pepper and n-hexane/acetonitrile partition was used for analysis of hulled rice and soybean. The instrumental conditions were tested for quantitation in GC/ECD and for confirmation in GC/MS. Recovery was in the range of 86~109% with RSD ${\leq}$10.2% and the quantitation limits (LOQ) of method were 0.025 mg/kg in all agricultural commodities. CONCLUSION: The result showed that the developed method can be used to determine picoxystrobin residue in agricultural commodities.

• Korean Journal of Food Science and Technology
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• v.45 no.5
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• pp.531-536
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• 2013

We developed a simple, sensitive, and specific analytical method for prometryn using gas chromatography-mass spectrometry (GC-MS). Prometryn is a selective herbicide used for the control of annual grasses and broadleaf weeds in cotton and celery crops. On the basis of high specificity, sensitivity, and reproducibility, combined with simple analytical operation, we propose that our newly developed method is suitable for use as a Ministry of Food and Drug Safety (MFDS, Korea) official method in the routine analysis of individual pesticide residues. Further, the method is applicable in clams. The separation condition for GC-MS was optimized by using a DB-5MS capillary column ($30m{\times}0.25mm$, 0.25 ${\mu}m$) with helium as the carrier gas, at a flow rate of 0.9 mL/min. We achieved high linearity over the concentration range 0.02-0.5 mg/L (correlation coefficient, $r^2$ >0.998). Our method is specific and sensitive, and has a quantitation limit of 0.04 mg/kg. The average recovery in clams ranged from 84.0% to 98.0%. The reproducibility of measurements expressed as the coefficient of variation (CV%) ranged from 3.0% to 7.1%. Our analytical procedure showed high accuracy and acceptable sensitivity regarding the analytical requirements for prometryn in fishery products. Finally, we successfully applied our method to the determination of residue levels in fishery products, and showed that none of the analyzed samples contained detectable amounts of residues.

• Analytical Science and Technology
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• v.23 no.2
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• pp.187-195
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• 2010

To assess health risk for the intake among residents after the Hebei Spirit oil spill, 16 Polycyclic Aromatic Hydrocarbons (PAHs) in seafood samples from oil contaminated bay were determined by Gas Chromatography-Mass Spectrometry (GC-MSD) and samples were personally collected and purchased by residents. Samples were hydrolyzed with KOH and extracted with methylene chloride. The extracted solution were cleaned up using silica/florisil column and 16 PAHs were eluted by methylene chloride : n-hexane (1:9) mixture and determined by GC-MSD in Selected Ion Monitoring (SIM) mode. The mean recoveries for 16 PAHs ranged from 79% to 85%. The 16 PAHs levels in 126 samples ranged from 0.17 to $6.04\;{\mu}g$/kg and the TEQBaP (Toxic EQuivalents) levels in 126 samples were calculated using benzo(a)pyrene toxic equivalency factor for individual 16 PAHs and ranged from 0 to $0.91\;{\mu}gTEQ$/kg. The average Benzo(a)pyrene dietary exposure of residents was $5.5{\times}10^{-8}\;mg/kg$ bw/day and the average PAHs chronic dietary exposure was $1.3{\times}10^{-5}\;mg$ TEQ/kg bw/day. The margin of exposure (MOE) and the excess cancer risk and were $1.8{\times}10^6$ and $9.8{\times}10^{-8}$, respectively. Therefore, the assessment result was considered as low concern for health risk.