• Korean Journal of Environmental Agriculture
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• v.31 no.1
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• pp.45-51
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• 2012

BACKGROUND: This study was carried out to establish pre-harvest residue limit of fungicides pyrimethanil and trifloxystrobin in persimmon, based on dissipation and biological half-lives of two fungicides residue. METHODS AND RESULTS: Both pyrimethanil and trifloxystrobin were extracted with acetonitrile, clean-up with $NH_2$ SPE cartridge and residue were analyzed by HPLC/DAD. Limit of Detection was 0.01 mg/kg. Average recovery were $81{\pm}1.62%$, $98{\pm}1.58%$ of pyrimethanil, and $91{\pm}2.94%$, $98{\pm}1.25%$ of trifloxystrobin at fortification levels at 0.1 and 0.5 mg/kg, respectively. CONCLUSION: The biological half-lives of pyrimethanil were 15.6 and 11.6 days at sprayed with recommended and double dosage, respectively. The biological half-lives of trifloxystrobin were 10.4 and 10.3 days at sprayed with recommended and double dosage, respectively. The pre-harvest residue limit of pyrimethanil and trifloxystrobin were recommended as 2.69 and 0.83 mg/kg for 10 days before harvest, respectively.

• 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.

• 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.

• Korean Journal of Environmental Agriculture
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• v.32 no.1
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• pp.84-93
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• 2013

BACKGROUND: This study was carried out to investigate the residual characteristics of insecticides used for Oriental Tobacco Budworm control and to establish the recommended pre-harvest residue limit leading to contribution in safety of paprika production. METHODS AND RESULTS: The recommended Pre-Harvest Residue Limits (PHRLs) of insecticides during cultivation of paprika were calculated from residue analyses of insecticides in fruits 1, 3, 5, 7, 10, 12, 15, 18 and 21 days after treatment. Paprika samples were extracted with QuEChERS method and cleaned-up with amino propyl SPE cartridge and PSA, and insecticide residues were analyzed either by HPLC/DAD or GLC/ECD. The limits of detection were 0.01 mg/kg for 5 insecticides. Average recoveries were $81.3{\pm}1.62%$-$98.3{\pm}1.58%$ of 5 insecticides at fortification levels of 0.1 and 0.5 mg/kg. The biological half-lives of the insecticides were 8.5 days for bifenthrin, 11.8 days for chlorantraniliprole, 16.8 days for chlorfenapyr, 7.1 days for lamda-cyhalothrin and 31.3 days for methoxyfenozide at recommended dosage, respectively. CONCLUSION(S): The pre-harvest residue limits for 10 days before harvest were recommended 1.05 mg/kg, 1.41 mg/kg, 0.93 mg/kg, 2.06 mg/kg and 1.08 mg/kg as bifenthrin, chlorantraniliprole, chlorfenapyr, lamda-cyhalothrin and methoxyfenozide, respectively. This study can provide good practical measures to produce safe paprika fruit by prevention of products from exceeding of MRLs at pre-harvest stage.

• Korean Journal of Environmental Agriculture
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• v.34 no.2
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• pp.120-127
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• 2015

BACKGROUND: Supervised residue trials were conducted to establish pre-harvest residue limit(PHRL), a criterion to ensure the safety of the pesticide residue in the crop harvest, of amisulbrom for winter-grown cabbage in two fields. Following to application of amisulbrom on the crop, time-course study was carried out to obtain the amisulbrom dissipation of statistical significance which enabled to calculate the predicted values of PHRL. METHOD AND RESULTS: During cultivation under greenhouse condition, samples of winter-grown cabbage were collected at 0, 1, 3, 5, 7 and 10 days after amisulbrom application, and subjected to residue analysis. Analytical method was validated by recoveries ranging 93.7~100.0% as well as limit of quantitation(LOQ) of 0.04 mg/kg. Amisulbrom residues in winter-grown cabbage gradually decreased as time elapsed. The dissipation rate of the residue would be affected by intrinsic degradation along with dilution by the cabbage growth. The decay pattern was well fitted by the simple first-order kinetics. CONCLUSION: Biological half-lives of amisulbrom in winter-grown cabbage ranged 3.7~4.1 days in two field conditions. Based on the regression of amisulbrom dissipation, PHRLs of amisulbrom in winter-grown cabbage were recommended as 8.86~9.47 and 4.21~4.35 mg/kg for 10 and 5 days before harvest, respectively.

• Horticultural Science & Technology
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• v.34 no.4
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• pp.644-654
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• 2016

Supervised residue trials for mandipropamid in Korean cabbage(Brassica campestris L.) were conducted to establish its pre-harvest residue limit (PHRL), a criterion to ensure the safety of the terminal pesticide residue during cabbage production. Tissues of Korean cabbage were collected at 0, 1, 3, 5, 7, and 10 days after mandipropamid application and subjected to residue analysis. The analytical method was validated by recoveries ranging from 88.2-92.2% at two levels (0.4 and $2.0mg{\cdot}kg^{-1}$), and a limit of quantitation (LOQ) of $0.04mg{\cdot}kg^{-1}$. Mandipropamid residues in Korean cabbage gradually decreased over time. The dissipation rate of the residue would be affected by intrinsic degradation of the compound along with dilution resulting from the fast growth of Korean cabbage. The decay pattern was well fitted by simple first-order kinetics. Biological half-lives of mandipropamid in Korean cabbage ranged from 3.9-4.0 days in two field conditions. Calculated by the regression curve of mandipropamid dissipation, the PHRLs of mandipropamid in Korean cabbage were recommended as 11.07-12.19 and $5.76-6.05mg{\cdot}kg^{-1}$ for 10 and 5 days prior to harvest, respectively.

• Korean Journal of Environmental Agriculture
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• v.36 no.1
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• pp.50-56
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• 2017

BACKGROUND: The present study was carried out to identify the residue patterns of insecticide pyridalyl and fungicide fluopicolide in watermelon and calculate the biological half-lives for establishing the pre-harvest residue limits (PHRLs). METHODSANDRESULTS:The watermelon samples for residue analysis were harvested 7 times during 0~10 days (Field 1) and 0~20 days (Field 2) after treatment of pesticides on watermelon in two different fields at the recommended dose, respectively. The residue analysis was conducted with HPLC/UVD. The method limit of quantitation (MLOQ) were set at 0.05 and 0.02 mg/kg, respectively, and overall mean recoveries were 81.2~90.5% for pyridalyl and fluopicolide. The residues in sample were stable for 43~47 days. The initial residue amount in field 1 and 2 were 0.12~0.16 mg/kg for pyridalyl and 0.23~0.24 mg/kg for fluopicolide, which were below maximum residue limit (MRL). The biological half-lives in field 1 and 2 were 26.9 and 17.9 days for pyridalyl and 16.6 and 94.2 days for fluopicolide, respectively. CONCLUSION: The PHRL for watermelon were estimated as 0.21 and 1.03 mg/kg for pyridalyl and flopicolide at 10 days before harvesting. The residue patterns of pyridalyl and fluopicolide were characterized by a very slow decrease of residue levels in watermelon.

• The Korean Journal of Pesticide Science
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• v.19 no.2
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• pp.81-87
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• 2015

The present study was aimed to predict the pre-harvest residue limits (PHRLs) of pyrimethanil (fungicide) and methoxyfenozide (insecticide) in grape, and to estimate their biological half-lives and residual characteristics. The pesticides were sprayed once on grape in two different fields 10 days before harvest. At the end of 0, 1, 2, 3, 5, 7 and 10 days after application, samples were harvested for further analysis. The residual pesticides were extracted with acetonitrile and partitioned with dichloromethane, and the high-performance liquid chromatography with diode array detector (HPLC/DAD) was employed for the residue analysis. The results obtained in the present study show that the limit of detection of both pesticides were found to be $0.01mg\;kg^{-1}$. The recoveries of these pesticides were ranged between 80.6% and 102.5% with coefficient of variation lower than 10%. The biological half-lives of both pesticides were observed in field 1 and field 2 which shows 7.7 and 7.4 days for pyrimethanil and 5.1 and 6.1 days for methoxyfenozide, respectively. Further, the PHRL of pyrimethanil and methoxyfenozide was found to be $8.90mg\;kg^{-1}$ and $5.51mg\;kg^{-1}$, respectively at 10 days before harvest. Consequently, the present study suggests that the residual amounts of both pesticides will be lower than the maximum residue limits (MRLs) when grape is harvested.

• The Korean Journal of Pesticide Science
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• v.18 no.1
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• pp.1-7
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• 2014

The present study was performed to investigate the pre-harvest residue limit (PHRL) of pesticides namely, metalaxyl-M and flusilazole in oriental melon, and to identify the biological half-life and characteristics of their residues. In this study, pesticides were sprayed once as single spray and double spray on oriental melon. The oriental melon samples were collected at 0, 1, 2, 3, 5, 7, 9 and 11 days before harvest and samples were extracted with QuEChERS method. The residues of both the pesticides were quantified using GC/NPD and LC/MS/MS. The limit of detection was found to be 0.02 mg/kg and 0.01 mg/kg and their recoveries were greater than 95% (95.7% ~ 103.2% for metalaxyl-M and 100.2% ~ 106.8% for flusilazole) for both pesticides. The biological half-lives of both metalaxyl-M and flusilazole were 12 days at single and double spray, respectively. The PHRL of metalaxyl-M and flusilazole was found 1.0 mg/kg and 0.3 mg/kg, respectively for 10 days before harvest. The results of the present study shows the residual level of both the pesticides metalaxyl-M and flusilazole in oriental melon were less than their maximum residual limits.

• The Korean Journal of Pesticide Science
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• v.17 no.4
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• pp.271-282
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• 2013

This is the result of pesticide residue monitoring certified Good Agricultural Practice (GAP) by national agricultural cooperative federation (NACF) from 2009 to 2012. NACF evaluated simultaneously 283 pesticide multi-analysis method with GC (ECD, NPD) and HPLC. 6,590 agricultural products were analyzed in this period. As the results 1) detected 20.27% in 2009, 23.42% in 2010, 28.07% in 2011 and finally 31.75% in 2012, respectively. There was the total detected pesticide residue in the agricultural products. The violated ratio of agricultural products were 2.25% in 2009, 1.82% in 2010, 1.67% in 2011 and 3.47% in 2012, respectively. 13 pesticides went over the maximum residue limits (MRLs); carbendazim was the predominant violation. 40 pesticides; endosulfan was the predominant detected pesticide did not registered respectively crops in Korea. Most agricultural products that were under the MRLs met the safety standard, however agricultural products that contain neither registered nor set up MRL any level for example endosulfan in strawberry. Agricultural products that go over the MRLs with permitted pesticides, for example carbendazim in apple, are rejected. Because of these intricacies continual observation and evaluation will be need during GAP agricultural cultivation.