• 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 Food Hygiene and Safety
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• v.33 no.4
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• pp.296-305
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• 2018

Spiroxamine, one of fungicides, is used to control powdery mildew in various crops and black yellow sigatoka in bananas. The major strength of spiroxamine is to control powdery mildew in various crops and bananas yellow sigatoka in bananas. The compound has shown a high level of activity, good persistence and crop tolerance. Besides powdery mildew, good control of rust, net blotch and Rhynchosporium diseases been indicated in cereals, together with a complementary activity against Septoria diseases. In 2017, the maximum residue limit (MRL) of spiroxamine established in Korea. According to Ministry of ood and rug afety) regulations, spiroxamine residues defined only parent compound. Thus, a analytical method is needed to estimate the residue level of the parent compound. The objective of this study was to develop and validate analytical method for spiroxamine in representative agricultural commodities. Samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interfering substances. The analyte were quantified and confirmed liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive-ion mode using multiple reaction monitoring (MRM). Matrix matched calibration curves were linear over the calibration ranges ($0.0005{\sim}0.1{\mu}g/mL$) for the analyte in blank extract with coefficient of determination ($r^2$) > 0.99. For validation purposes, recovery studies will be carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries 70.6~104.6% with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges in the Codex guidelines (CAC/GL40, 2003) and MFDS guidelines. proposed analytical method be used as an official analytical method in the Republic of Korea.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.174-184
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• 2015

In the present study, the metabolism of [$^{14}C$]butachlor was investigated in rice plant according to the OECD test guideline No. 501. [$^{14}C$]Butachlor was treated as granule to paddy water by application of 1.5 kg ingredient (a.i.)/ha at the 3~4 leave stage of rice plant. At 85 days after treatment (DAT), samples of panicle, foliage, and roots were taken for radioactivity analysis. Upon harvest at 126 DAT, rice plants were separated into brown rice, husk, straw, and root parts. Amounts of total radioactivity absorbed by rice plant ranged from 8.6 to 9.8% of applied radioactivity (AR). Total radioactive residues (TRRs) of rice plant at 126 DAT was the highest as 4.0421 mg/kg (7.3% AR) in the straw followed by 1.4595 mg/kg (2.4% AR) in the root, 0.7257 mg/kg (0.1% AR) in the husk. The lowest level recording 0.1020 mg/kg (0.1% AR) was found in brown rice. Each part was extracted with various solvents and solvent/water mixtures. Greater than 70% of TRRs was readily extractable from foliage, panicle, husk and straw. Only 34.0% of the brown rice and 43% of root based on TRRs were extractable showing that the residues were completely assimilated in the plant tissue. The level of non-extractable radioactivity was ranged from 26.2 to 66.0% of TRRs. From this study, five tentative major metabolites (M1, M2, M3, M4 and M5) were observed in rice extracts. Among the metabolites, 2,6-diethylaniline assigned as M4 was identified in rice plant by comparing to retention time of reference standard. Un-metabolized butachlor was not detected in any fractions. In soil extracts, N-(butoxymethyl)-N-(2,6-diethyl phenyl)acetamide, 2,6-diethylaniline, M2, M3 and M5 were observed. And the concentration of butachlor was low level (ca. 0.03 mg/kg).

• Korean Journal of Food Science and Technology
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• v.42 no.1
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• pp.1-7
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• 2010

To revise the dithiocarbamates residue analysis method and survey the residues in agricultural products that were treated with these fungicides in Korea, we purchased 20 types of foodstuffs (rice, potato, cabbage, apple etc.) from markets in five major cities. 236 samples of the purchased foodstuffs were then analyzed for the presence of dithiocarbamates by HPLC/UV and HPLC/APCI-MS. The $R^2$, LOD and LOQ in the range of 0.5-107.3 mg/L were as follows: DCC: y=174.34x+18.315, $R^2=0.9999$, 0.01 mg/L, and 0.04 mg/L; EBDC: y=227.38x-14.715, $R^2=1.0000$, 0.01 mg/L and 0.02 mg/L; PBDC: y=38.46x-21.412, $R^2=0.9999$, 0.04 mg/L, and 0.1 mg/L; ETU: y=52.752x-4.4819, $R^2=0.9998$, 0.02 mg/L and 0.03 mg/L; PTU: y=128.28x+4.4624, $R^2=0.9998$, 0.02 mg/L, and 0.04 mg/L. The levels of DDC, EBDC, PBDC, ETU and PTU in 20 agricultural products fortified to 10.0-107.3 mg/L ranged from 61.7-117.5%, 65.3-110.1%, 61.5-109.6%, 69.3-116.3% and 70.2-97.2%, respectively. Overall, dithiocarbamates were detected in 100 samples and the detection ratio was 42.4%. Among these, only 3 samples (1.3%) of Lycii fructus had residue levels that were above the action limits, while the remaining samples (233 samples) contained levels of dithiocarbamates below the detection limit or below the Korea MRLs (Maximum Residue Limits).