• Korean Journal of Environmental Agriculture
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• v.31 no.2
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• pp.157-163
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• 2012

BACKGROUND: For the safety of imported agricultural products, the study was conducted to develop the analytical method of unregistered pesticides in domestic. The analytical method of 6 pesticides, chlorthal-dimethyl, clomeprop, diflufenican, hexachlorobenzene, picolinafen, and propyzamide, for a fast multi-residue analysis were established for two different type crops, orange and brown rice by GC-ECD and confirmed by mass spectrometry. METHODS AND RESULTS: The analytical method was evaluated to limit of quantification, linearity and recoveries. The crop samples were extracted with acetonitrile and performed cleanup by liquid-liquid partition and Florisil SPE to remove co-extracted matrix. The extracted samples were analyzed by GC-ECD with good sensitivity and selectivity of the method. The limits of quantification (LOQ) range of the method with S/N ratio of 10 was 0.02~0.05 mg/kg for orange and brown rice. The linearity for targeted pesticides were $R^2$ >0.999 at the levels ranged from 0.05 to 10.0 mg/kg. The average recoveries ranged from 74.4% to 110.3% with the percentage of coefficient variation in the range 0.2~8.8% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in brown rice. And the average recoveries ranged from 77.8% to 118.4% with the percentage of coefficient variation in the range 0.2~6.6% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in orange. Final determination was by gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM) to identify the targeted pesticides. CONCLUSION: As a result, this developed analytical method can be used as an official method for imported agricultural products.

• The Korean Journal of Pesticide Science
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• v.18 no.3
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• pp.123-129
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• 2014

The present work was aimed to determine the pre-harvest residue limits (PHRLs) and the safety management of commonly used pesticides namely buprofezin and penthiopyrad on oriental melon (Cucumis melon var. makuwa). In this study, the buprofezin (diluted two thousand fold) and penthiopyrad (diluted four thousand fold) were sprayed single time on oriental melon in the cultivation areas Sangju (site 1) and Sungju (site 2). Oriental melon were randomly collected from the both areas at the end of 0 (2 hours after pesticides spaying), 1, 2, 3, 5, 7, 9 and 10 days. For analysis, each samples were partitioned twice (80 and 70 mL) with dichloromethane and purified by florisil SPE cartridge. Finally, the residual amounts of both pesticides in all samples were analyzed using gas chromatography/nitrogen phosphorus detector (GC/NPD). In this study, the method limit of quantification (MLOQ) for both buprofezin and penthiopyrad in oriental melon was found to be $0.01mg\;kg^{-1}$ and their recovery levels were 91.1~98.6% and 90.0~104.6%, respectively. Further, the calculated biological half-life for buprofezin and penthiopyrad in oriental melon were 3.9 and 3.5, and 3.0 and 2.7 days in site 1 and 2, respectively. The results of this study found that the PHRLs for buprofezin and penthiopyrad were 4.24 and $2.31mg\;kg^{-1}$, respectively at 10 days before harvest. Consequently, the present study suggest that the residual amounts of both pesticides will be lower than the maximum residue limits (MRLs) when oriental melon is harvested.

• 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 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.

• Korean Journal of Food Science and Technology
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• v.36 no.4
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• pp.688-691
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• 2004

Concentrations of PAHs [benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene, indeno(1,2,3-c,d)pyrene] in vegetable oils and fats available in Korean market were estimated. Involved methodology were liquid-liquid partition, purification on Sep-Pak Florisil Cartridges, and high performance liquid chromatography using fluorescence detector. Overall recoveries for eight PAHs spiked into vegetable oils and fats ranged from 68.2 to 101.5%, averaging 85.4%. Mean levels of benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene, and indeno(1,2,3-c,d)pyrene in vegetable oils and fats were 0.53, 0.82, 0.50, 0.18, 0.35, 0.16, 0.31, and $0.44{\mu}g/kg$, respectively.

• 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 Food Science and Technology
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• v.31 no.4
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• pp.931-937
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• 1999

Styrene dimers and trimers from polystyrene cup noodle containers were analyzed by GC and GC/MS extracted with various simulants. For the quantitation of styrene dimers and trimers, 1,3-diphenylpropane (DP) and benzyln-butyl phthalate (BBP) were chosen as the standards. The results showed that the average of the styrene dimers in the containers was 603 ppm, and that of trimers was 5731 ppm. Four styrene dimers, including 1,2-diphenyl-cyclobutane, were identified as well as seven trimers such as 2,4,6-triphenyl-l-hexene. The migration of the styrene dimers and trimers, from the cup noodle containers of polystyrene into foods, was conducted using simulants including boiling water as well as soybean oil and n-heptane. In addition to, the analysis of each migrated styrene was also performed filled with boiling water into noodle and soup after certain time (5, 10, 20, 30 min). The results showed that the migration of styrene dimers and trimers from cup noodle containers was not detected in the case of using boiled water or soybean oil as a simulant, while styrene dimers and trimers were detected 1.18 ppm and 14.21 ppm, respectively, when heptane was adopted as a simulant. In the case of filling with boiled water into noodle and soup, both styrenes were not detected at 5 min and 10 min, however, some samples standing for 20 min released styrene dimers and trimers as much as 0.009 ppm, and 0.019 ppm for 30 min.

• 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.

• 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 Food Science and Technology
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• v.41 no.3
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• pp.339-344
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• 2009

Concentrations of polycyclic aromatic hydrocarbon (PAH) in processed chestnut products were determined by HPLC/FLD. The methodology involved procedures of sonication with water, extraction with hexane, and clean-up on a Sep-pak florisil cartridge. The PAH limits of detection (LOD) and limits of quantitation (LOQ) ranged from 0.012 to 0.382 ${mu}g/kg$ and from 0.042 to 1.273 ${mu}g/kg$, respectively. The coefficients of variation for intra- and inter-day assays were 0.02-4.48% and 0.37-9.83%, respectively, and the accuracies were 81.95-125.44% and 79.89-116.53%, respectively. The overall recoveries for eight PAHs spiked into the processed chestnut products ranged from 87.83 to 100.56%. As a result, PAH contents were not detected in the processed chestnut products.