• Korean Journal of Environmental Agriculture
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• v.37 no.3
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• pp.213-220
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• 2018

BACKGROUND: This study was carried out to determine characteristics of residual pesticides in time-dependent manner and calculate half-lives of the residual pesticides in fresh and dried Chinese matrimony vine. In addition, processing factors were calculated based on the residual concentrations in them. METHODS AND RESULTS: The test pesticides, etofenprox and fenitrothion, were sprayed onto the Chinese matrimony vine plants at once or twice (at seven-day interval) and then samples were collected at 0 (after 3 hours), 1, 3, 5 and 7 days after the last spraying. Dried samples were prepared in hot-air drying oven at $60^{\circ}C$ for 48 hours until water content of less than 20%. Residual concentrations of etofenprox in fresh and dried samples decreased by 54.0-60.9% after 7 days of the last pesticide-application. In case of fenitrothion, the concentrations were found to have decreased by 69.2-76.5%. Processing factors of etofenprox were 2.6-3.0 for the one-time spraying and 2.5-3.0 for the two-time spraying and those of fenitrothion were found to be 1.5-22 for the one-time spraying and 1.6-2.0 for the two-time spraying. First half-lives of etofenprox and fenitrothion in fresh and dried samples ranged from 5.0 to 6.3 and from 3.4 to 4.0 days, respectively. The third half-lives were found to be 15.0-18.9 and 10.2-12.1 days, respectively. CONCLUSION: Residual concentrations of the tested pesticides in the studied crop decreased, but those in the dried samples appeared to have increased. In addition, processing factor and half life were constant regardless of spraying times.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.191-198
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• 2019

This study investigated the residual characteristics of bifenthrin and chlorothalonil in crown daisy and suggested pre-harvest residue limits (PHRLs) based on their dissipation patterns and biological half-lives. The samples for residue analysis were harvested at 0 (3 hr), 1, 3, 5, 7, 9, 11, 13, 15, 18, 22 and 26 days after treatment, and analyzed by $GC/{\mu}-ECD$ and TOF/MS. The limit of quantitation (LOQs) of bifenthrin and chlorothalonil were 0.0046 mg/kg and 0.0007 mg/kg, respectively. Recoveries ranged from $88.67{\pm}7.97%$ and $99.90{\pm}16.03%$, showing that this method is appropriate for the analysis of the pesticide residues in crown daisy. Being well within first order kinetics, the biological half-lives of the pesticide residues in crown daisy were 9.63 days for bifenthrin and 6.54 days for chlorothalonil. The PHRLs of bifenthrin and chlorothalonil were recommended as 11.70 mg/kg and 24.10 mg/kg for 26 days before harvest, respectively.

• The Korean Journal of Pesticide Science
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• v.17 no.4
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• pp.307-313
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• 2013

This study was carried out to investigate the residual characteristics of fungicide azoxystrobin and difenoconazole in Prunus mume fruits, and establish pre-harvest residue limits (PHRL) based on dissipation and biological half-lives of fungicide residues. The fungicides were sprayed onto the crop at recommended dosage once and 3 times in 7 days interval, respectively. The samples were harvested at 0, 1, 2, 4, 6, 8, 10, 12 and 14 days after treatment. These residual pesticides were extracted with QuEChERS method, clean-up with $NH_2$ SPE cartridge, and residues were analyzed by HPLC/DAD and GLC/ECD, respectively. Method quantitative limits (MQL) of azoxystrobin were 0.03 mg $kg^{-1}$ and of difenoconazole were 0.006 mg $kg^{-1}$. Average recovery were $93.2{\pm}2.49%$, $85.5{\pm}1.97%$ for azoxystrobin at fortification levels at 0.3 and 1.5 mg $kg^{-1}$, and $100.8{\pm}6.74%$, $87.6{\pm}9.92%$ for difenoconazole at fortification levels at 0.06 and 0.3 mg $kg^{-1}$, respectively. The biological half-lives of azoxystrobin were 5.9 and 5.2 days at recommended dosage once and 3 times in 7 days interval, respectively. The biological half-lives of difenoconazole were 9.3 and 8.0 days at recommended dosage once and 3 times in 7 days interval, respectively. The PHRL of azoxystrobin and difenoconazole were recommended as 5.32 and 1.64 mg $kg^{-1}$ for 10 days before harvest, respectively.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.248-254
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• 2015

Uptake of the triazole fungicides, fluquinconazole and tetraconazole from shoot part of onion was assessed by determining residual amounts of applied fungicides in edible and shoot parts of onion after the foliar application. Combined product of fluquinconazole and tetraconazole (14:7, v/v) as a 21% active ingredient of suspended emulsion formulation was diluted at ratio of 500 and 200 times and sprayed on the shoot part of onion after sealing its root part with absorbent paper. At 10 days after the pesticide application, fluquinconazole residue in the shoot part was the greatest as 5.2 mg/kg at 200 times-dilution treatment, while tetraconazole residue in this part was the smallest as 1.2 mg/kg at 500 times-dilution treatment. On the other hand, the pesticide residues in edible parts of onion at all the treatments were less than limits of detection, 0.01 mg/kg. However, fluquinconazole residues in the edible part of onion divided into three groups such as 1st, 2nd, and 3rd layers were detected at concentrations of 0.04 or 0.24 mg/kg, and these results show the different distribution of pesticides in onion depending on divided layers. In addition, chopped onions were soaked in pesticide solutions prepared with dilution of 1,000 times, cooked using three food processing types such as boiling, stir frying, and pickling, and the pesticide residues in them were analyzed. The analyzed results showed the largest pesticide dissipation in onion followed boiling process (76.9~92.6%).

• Korean Journal of Environmental Agriculture
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• v.33 no.4
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• pp.290-297
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• 2014

BACKGROUND: The current study purposed to analyse the dissipation levels of a neonicotinoid insecticide and clothianidin in paddy and upland soils and clarify the effects of soil moisture on degradation and persistence of the insecticide. METHODS AND RESULTS: In order to achieve the research purposes, clothianidin 8% SG was applied to the paddy and upland fields at the rate of 0.024 kg a.i./10a, while the analytical standard was treated at 0.25 mg/kg soil under laboratory conditions. Based on the multiple first-order kinetics, total clothianidin in soils was dissipated with $DT_{50}$ of 6.7-16.1 and 6.9-8.2 days in the paddy and upland fields, respectively, whereas the figures under the laboratory condition became larger showing 56.3 and 19.6 days. CONCLUSION: As affected by soil moisture, some differences in degradative pathways were observed. Flooding of soil caused evidently demethylation and delayed cyclization of a major metabolite, thiazolylmethylguanidine (TMG) and methylaminoimidazole(MAI), compared to the aerobic upland condition. More than 80% and 50% of the parent compound was dissipated by the 24th day after the final application in both soils and, transformation products had constituted most of soil residues after that.

• The Korean Journal of Pesticide Science
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• v.15 no.3
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• pp.269-277
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• 2011

Recent outbreak of new diseases and pests which were introduced from abroad, seriously hampered both quality and safety of paprika fruits. This study has been carried out to aid an establishment of guideline for safe use of pesticides and reduction of their residues on paprika. Systemic fungicides boscalid and pyraclostrobin of either mixed (a.i.; 13.6+6.8%) or single (a.i.; 47 and 18.8%, respectively) water dispersible granule formulation(WG) products were sprayed with recommended or double dosage on paprika grown in green house at March and June. To draw pre-harvest residue limit, residues of each fungicide were analyzed from fruits collected eight times from 18 to 1 day pre-harvest. The biological half-lives of both boscalid and pyraclostrobin in mixed formulation in March and June were slightly shorter than those of single formulation which ranged from 14.4 to 20.1 days. Residue levels of both fungicides of single formulation in fruits in June were about one lower compared to those in March. However, application of double dosage frequently exceeded MRLs from fruits grown both seasons. These results showed that residue levels on fruits persisted longer period of time, more than two weeks, and so the case applied in winter season. The dissipation of fungicides on leaves and fruits was compared. The distribution of both fungicides in leaves was 20-200 times higher than that of fruits and persisted up to 18 days of pre-harvest period at the concentration of 10-40 ${\mu}g\;g^{-1}$. This study indicated that the mixed formulation product exhibited low residues in fruits, but high and long enough to pathogen growth in leaves.

• The Korean Journal of Pesticide Science
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• v.13 no.1
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• pp.28-38
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• 2009

An extrapolation of residue data of seven commonly used pesticides namely bifenthrin, chlorothalonil, cypermethrin, diazinon, fenvalerate, phenthoate and procymidone on a total of 22 minor crops has been carried out in an experimental field trial. The pesticides were applied to 11 leafy-, 5 root- and 6 stem-crops grown in the experimental green-house and the crops and plants were randomly collected at 1, 3, 5, 7 days after application. The average recoveries of applied pesticides were ranged from 72.0 to 117.0% in leafy crops, from 81.3 to 105.0% in stem crops and from 70.1 to 108.1% in the root-crops. Limits of detection (LODs) were 0.005-0.1 mg/kg in the leafy crops and 0.001-0.005 mg/kg in both the stem & root crops. Based on the results of residual dissipation pattern and their morphology, all crops were classified into high and low residual groups. The results showed that it might be possible to extrapolate residual data of stem-crops to root-crops within the same group. Crops that have currently no registered pesticide for use, would be possible to use the pesticides which are already been registered for the similar crops.

• Journal of Applied Biological Chemistry
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• v.59 no.4
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• pp.331-336
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• 2016

Analytical methods for methiozolin in soil, water and turfgrass were established and dissipation patterns of methiozolin in soil and turfgrass were elucidated. Analysis was done using a high performance liquid chromatography with an ultra violet detector at the wavelength of 280 nm after extraction with acetone, liquid-liquid partition with dichloromethane, and a solid phase extraction purification. Limit of determination and Limit of quantitation were 1.0, 0.5, 1.0 ng, and 0.001, 0.1, 0.01 mg/kg for water, turfgrass, and soil, respectively. Recovery rates of methiozolin from soil, water, and turfgrass were ranged 87.5~111.3, 92.8~97.4, and 78.2~98.5 %, respectively. The turfgrass and soil samples were collected at 0, 1, 4, 7, 14, 30, 45, and 60 after spray on green area in golf course. Residues of methiozlolin were not translocated to lower soil layer but detected only in turfgrasses and root area of turfgrass. Half-lives of methiozolin in turfgrass were 10.7 days and 8.8 days in soil from root area.

• Bulletin of the Korean Chemical Society
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• v.32 no.12
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• pp.4265-4269
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• 2011

A method based on ethyl acetate extraction and gas chromatography with tandem mass spectrometry was developed for determining tetraconazole residues in fruits and vegetables. A 10 g homogenized sample was mixed with 10 mL ethyl acetate, shaken vigorously for 3 min, stored at $-20^{\circ}C$ for 15 min, and then vortexed vigorously for 1 min; 1 g NaCl and 4 g anhydrous $MgSO_4$ were added. The clean-up was carried out by applying dispersive solid-phase with 150 mg $MgSO_4$and 50 mg primary secondary amine. Three precursor product ion transitions for tetraconazole were measured and evaluated to provide the maximum degree of confidence. Average recoveries in fruits and vegetables at three levels (0.005, 0.05 and 0.5 mg/kg) ranged from 85.53% to 110.66% with relative standard deviations ($RSD_r$) from 1.3% to 17.5%. The LODs ranged from 0.002 to 0.004 ${\mu}g$/kg, and LOQs ranged from 0.006 to 0.012 ${\mu}g$/kg. This method was also applied to determine tetraconazole residue in cucumber dissipation experiment under field conditions. The half-lives of tetraconazole in cucumber were in the range of 2.1-3.1 days.

• Toxicological Research
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• v.24 no.3
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• pp.207-212
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• 2008

Pesticide residues play several key roles as environmental and food pollutants and it is crucial to develop a method for the rapid determination of pesticide residues in environments. In this study, a simple, effective, and sensitive method has been developed for the quantitative analysis of methoxyfenozide in water and soil when kept under laboratory conditions. The content of methoxyfenozide in water and soil was analyzed by first purifying the compound through liquid-liquid extraction and partitioning followed by florisil gel filtration. Upon the completion of the purification step the residual levels were monitored through high performance liquid chromatography(HPLC) using a UV absorbance detector. The average recoveries of methoxyfenozide from three replicates spiked at two different concentrations and were ranged from 83.5% to 110.3% and from 98.1% to 102.8% in water and soil, respectively. The limits of detection(LODs) and limits of quantitation(LOQs) were 0.004 vs. 0.012 ppm and 0.008 vs. 0.024 ppm, respectively. The method was successfully applied to evaluate the behavioral fate of a 21% wettable powder(WP) methoxyfenozide throughout the course of 14 days. A first-order model was found to accurately fit the dissipation of methoxyfenozide in water with and a $DT_{50}$ value of 3.03 days was calculated from the fit. This result indicates that methoxyfenozide dissipates rapidly and does not accumulate in water.