• The Korean Journal of Pesticide Science
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• v.17 no.4
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• pp.314-334
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• 2013

This study explored an efficient modified Quick, Easy, Cheap, Effective, Rugged and safe (QuEChERS) method combined with liquid chromatography-electrospray ionization with tandem mass spectrometric detection for the analysis of residues of 76 pesticides in brown rice, barley and corn including acidic sulfonylurea herbicides. Formic acid (1%) acid in acetonitrile and dispersive solid phase extractions used for extraction of pesticides and clean-up of the extract respectively. Two fortified spikes at 50 and 200 ng $g^{-1}$ levels were performed for recovery test. Mean recoveries of majority of pesticides at two spike levels ranged from 73.2 to 132.2, 80.9 to 136.8, 66.6 to 143.5 for brown rice, barley and corn respectively with standard error (CV) less than 10%. Good linearity of calibration curves were achieved with $R^2$ > 0.9907 within the observed concentration ranged. The modified method also provided satisfactory results for sulfonylurea herbicides. The method was applied to the determination of residues of target pesticides in real samples. A total of 26 pesticides in 36 out of 98 tasted samples were observed. The highest concentration was observed for tricyclazole at 1.17 mg $kg^{-1}$ in brown rice. This pesticide in two brown rice samples exceeded their MRLs regulated for rice in republic of Korea. Except tricyclazole none of the observed pesticides' concentration was higher than their MRLs. The results reveal that the method is effectively applicable to routine analysis of residues of target pesticides in brown rice, barley and corn.

• Korean Journal of Environmental Agriculture
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• v.38 no.4
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• pp.281-290
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• 2019

BACKGROUND: As the demand for strawberries increases, people are paying attention to food safety in strawberry, especially pesticide residues. To remove the pesticides from strawberry, various washing and processing technique in households are additionally required. METHODS AND RESULTS: Strawberries were washed with water, detergent, alcohol, and ultrasonication and processed to strawberry jam. The mean reduction efficiency according to the washing solvent and method was found to be higher in the order of detergent (42.5%) > alcohol (41.7%) > water (41.3%) > ultrasoniation with alcohol (40.2%) > ultrasoniation with water (38.6%) > ultrasoniation with detergent (36.9%), but there was no significant difference among the treatments. The residue levels of pesticides during processing to jam decreased by 11.9-94.4% for etoxazole, fluopyram, procymidone, spiromesifen, and prochloraz, while the other pesticides were concentrated by boiling, or rather increased by 11.8-40.2%. However, when the residue levels were converted to residual amounts in consideration of the change in weight after processing, the residual amounts of the tested pesticides were reduced by 59.8-98.4% during processing. The processing factor (PF) were different for each pesticide, but PFs were < 1 for all washing solvents and methods, and 0.06-1.40 when processed into jam. CONCLUSION: To ensure the consumption of pesticide-free strawberry, the most efficient washing method is to immerse the strawberry in fresh water for few minutes, followed by rinsing them under running water.

• The Korean Journal of Pesticide Science
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• v.17 no.3
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• pp.178-184
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• 2013

Residual toxicity test to honeybee was conducted to evaluate an indirect effects on honeybee after planting hole application of systemic insecticides which were highly toxic to honeybee (Apis mellifera). In this study, It was applied three application rates in the planting hole by three systemic insecticides, dinotefuran GR, imidacloprid GR and clothianidin GR at planting time of tomato. Residual analysis of foliage was carried out after periodic sampling the foliage and investigated the effects of exposed honeybee on the tomato foliage. The honeybee mortality by dinotefuran residues on the foliage was shown almost 100% at 7 days after treatment and decreased 17 days after treatment. The maximum mortality of honeybee by imidacloprid residues on the foliage was 44 ~ 72%. But the effect of pesticide lasted for 18 days and then decreased. The honeybee mortality by clothianidin residues on the foliage was 100% at 7 days after treatment and decreased 14 days after treatment. A tendency of the honeybee mortality and residue in foliage showed a similar character as time goes by. The residues in tomato foliage decreased gradually after 14 days by vigorous growth of tomatoes and the toxic effect of honeybee was significantly decreased after 21 days in actual usage of the treatment.

• Korean Journal of Environmental Agriculture
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• v.38 no.4
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• pp.338-351
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• 2019

BACKGROUND: To investigate distribution and seasonal variation of concentration and flux of pesticides in Han river basin, water samples were examined at 24 sites in 2012 and 2014. METHODS AND RESULTS: Water samples were collected four times per year and subjected to liquid-liquid partition extraction followed by GC-ECD/NPD analysis. Of fifteen pesticides detected, iprobenfos, diazinon, isoprothiolane, endosulfan sulfate and oxadiazon were detected in a higher frequency, while fenoxanil, carbofuran, fenitrothion, butachlor and metolachlor were only detected in a sample. Pesticides with high occurrences, iprobenfos, diazinon, isoprothiolane, endosulfan sulfate and oxadiazon were detected in residue level of 0.01-0.46, 0.01-0.24, 0.03-0.85, 0.02-0.06 and 0.05-0.24 ㎍/L, respectively. Carbofuran and acetanilide herbicides were found at lower frequencies, but their concentrations were one order of magnitude higher than those of the others. CONCLUSION: Discharge of pesticides in downstream area were mainly contributed from rice farming and suburban horticulture, while pesticide occurrences in upstream area, such as Donggang river basin were caused by highland agriculture for cabbage and potato production. Despite the influx of pesticides from tributaries through intensive agriculture areas, pesticide concentration in the main stream water was low due to the dilution effect from the upstream. Therefore, the water quality was considered to be good at the most downstream, the effluent of Paldang dam.

• The Korean Journal of Pesticide Science
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• v.20 no.4
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• pp.341-348
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• 2016

Residual patterns of fungicides fludioxonil and metconazole applied 2 or 3 times on wheat were investigated with consideration for their distribution rates in each compartment of wheat. Wheat samples collected at harvesting day were divided into three compartments such as grain, hull and straw, and the pesticide residue analysis was individually carried out to such compartments of wheat. The analytical methods of fungicide residues in wheat were acceptable, with recoveries of 84.3 to 113.3% and correlation coefficients of 0.1 to 4.7%. Due to the systemic characteristics, the residual amounts of metconazole in the grain part of wheat were greater as 0.13~0.17 mg/kg than those amounts (0.01-0.03 mg/kg) for fludioxonil. To absolute residue amounts of the fungicides in one wheat plant, their distribution rates in each compartment of wheat were the highest in straws (68.5-70.7%), followed by hulls (29.0-31.0%) and grains (0.2-0.8%).

• The Korean Journal of Pesticide Science
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• v.13 no.3
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• pp.127-132
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• 2009

The purpose of this study is to examine changes in the pesticides residues in pepper powder by storage conditions. Analysis of pesticide residues was performed using multiresidue analytical methods and the number of pesticides detected from 60 pepper powders was 7 pesticides such as cypermethrin, fenvalerate, kresoxim-methyl, chlorpyrifos, chlorfenapyr azoxystrobin, tebuconazole. The concentrations of cypermethrin and tebuconazole were exceeded their maximum residue limits (MRLs). The degradation patterns of pesticides at $-5^{\circ}C$ were compared to those at $20^{\circ}C$ and $4^{\circ}C$. Without reference to storage temperature, degradation rates of azoxystrobin and fenvalerate were above 80%. Degradation rate of chlorpyrifos was 47% at storage $4^{\circ}C$, $20^{\circ}C$ and 34% at storage $-5^{\circ}C$. During each storage peroid, the degradation patterns were more lower at $-5^{\circ}C$ than at $20^{\circ}C$ and $4^{\circ}C$.

• Korean Journal of Organic Agriculture
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• v.19 no.1
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• pp.121-134
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• 2011

For this study, Smilex powder, a pesticide, was sprayed on the Altari radish, and then underground water, Chitosan solution (${\times}$500), and wood vinegar solution (${\times}$1000) were evenly sprayed on the Altari radish respectively. Samples of Altari radishs for residual pesticide analysis were taken two hours, 1 day, 7 days, and 15 days after treatments, and the detectable concentration and degradability of procymidone, the pesticide residue, were measured. The results obtained are as follows: 1. When detectable concentration of procymidone within the altari radish was measured, treatment plots sprayed with underground water, Chitosan solution (${\times}$500), and wood vinegar solution (${\times}$1000) were found to show lower detectable concentration than the non-treatment plot which was sprayed with pesticide only. Especially, the treatment plots sprayed with Chitosan solution (${\times}$500), and with wood vinegar solution (${\times}$1,000) showed lower values than the average. 2. When the degradability of procymidone within the Altari radish was measured, the plot treated with Chitosan solution (${\times}$500) and the plot treated with wood vinegar solution (${\times}$1,000) were found to have relatively higher degradability of procymidone. There were not much differences among testing materials in the degradability of residual pesticides. However, the plot treated with Chitosan solution (${\times}$500) showed higher degradability. In terms of average degradability with time, degradability increased sharply 7 days after the foliar application of testing materials. 3. When the daily far-sighted view survey was conducted in order to find out growth disorder and damage on the Altari radish plants by the treatment of un-derground water, Chitosan solution (${\times}$500), and wood vinegar solution (${\times}$1,000), no symptomatic physiological disorders was observed on all the plants tested during the whole growing season at the tested concentration level.

• Journal of Applied Biological Chemistry
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• v.63 no.1
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• pp.51-60
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• 2020

This study was conducted to investigate changes in pesticide residues in eggplant and lettuce during washing and cooking processes after application with azoxystrobin. Eggplant was processed with running washing, steaming, and stir-frying, and lettuce was processed with soaking washing, running washing, soaking and running washing, ultrasonic cleaning, and blanching. The limit of quantitation of GC analysis of azoxystrobin was 0.01 mg/kg and the recovery rate was 84.7-109.5%. The azoxystrobin processing factors (PFs) and reduction rates in eggplant and lettuce were calculated and the results were as follows. In the case of eggplant, the azoxystrobin PF and reduction rate of running washing were 0.29 and 71.1%, respectively, those of steaming were 0.32 and 68.0%, respectively, and those of stir-frying were 0.24 and 75.7%, respectively. In the case of lettuce, the azoxystrobin PF and reduction rate of soaking washing were 0.25, 75.3%, those of running washing were 0.61 and 38.9%, respectively, those of soaking and running washing were 0.32, 68.0%, those of ultrasonic cleaning were 0.47 and 53.1%, respectively, and those of blanching were 0.26 and 73.6%, respectively. It could be identified that pesticide residues in eggplant and lettuce can be effectively reduced through washing and cooking processes and that most of pesticide residues were removed when cooking processes were undergone after washing. Therefore, azoxystrobin PFs after washing and processing can be provided as basic data for risk assessment.

• The Korean Journal of Pesticide Science
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• v.18 no.4
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• pp.296-313
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• 2014

A QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) multiresidue method was developed for the simultaneous analysis of 124 pesticides in soil by LC-MS. The procedure involved liquid extraction of soil immersed with 0.2N $NH_4Cl$ by acetonitrile with 1% acetic acid, followed by anhydrous $MgSO_4$ and sodium acetate, and dispersive SPE cleanup with $MgSO_4$, primary secondary amine (PSA) and $C_{18}$. The extracts were analyzed with LC-MS/MS in ESI positive mode. Standard calibration curves were made by matrix matched standards and their correlation coefficients were higher than 0.99. Recovery studies for the validation were carried out using two type soils, loam and sandy loam, at four concentration levels (0.005, 0.01, 0.02, and 0.1 mg/kg). The recoveries of pesticides were in the range of 70-120% with < 20% RSD except 4 pesticides, Benfuracarb, Ethiofencarb, Pymetrozine, and Pyrethrin. This result indicated that the method using QuEChERS and LC-MS/MS could be applied for the simultaneous determination of pesticide residues in soils.

• The Korean Journal of Pesticide Science
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• v.20 no.2
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• pp.104-127
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• 2016

A new analytical method has been developed to determine 320 pesticides in apple and rice. The extraction of pesticides was carried out based on QuEChERS sample extraction, and determination was performed using LC-MS/MS and GC-MS/MS. 320 pesticides were selected for experiments. 251 and 110 pesticides among them were analysed by LC-MS/MS and GC-MS/MS, respectively. 41 pesticides of them were analyzed by both GC-MS/MS and LC-MS/MS. Among pesticides analysed by LC, 242 pesticides (96% of total number) in apple and 237 pesticides (94% of total number) in rice showed recoveries in the range of 70~120% with RSD ${\leq}20%$. In case of pesticides analyzed by GC-MS/MS, 103 pesticides (94% of total number) in apple and 83 pesticides (76% of total number) in rice were successfully validated. These results indicated that LC-MS/MS and GC-MS/MS analysis with the QuEChERS sample preparation can be partly applied to multi-residue pesticides in agricultural products.