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

• Korean Journal of Environmental Agriculture
• /
• v.35 no.4
• /
• pp.278-285
• /
• 2016

BACKGROUND: Uptake patterns of ${\alpha}$-, ${\beta}$-isomers and sulfate metabolite of endosulfan (ED) by radishes grown in treated soils with ED concentrations of 2 and 10 mg/kg were investigated to establish soil management guidelines for ensuring the safety of radishes from ED residues. METHODS AND RESULTS: All samples of soils and radish plants separated into shoot and root parts were analyzed for ED residues using a gas-chromatography mass spectrophotometer, and the results were used to calculate the bioconcentration factor (BCF), indicating the ratio of ED concentrations between radishes and soils. During the experimental period, uptake and distribution rates of ED-sulfate in radishes were the highest, followed by ${\alpha}$- and ${\beta}$-ED. The BCF values to initial ED concentrations in soils were greater for root parts (0.0077 to 0.2345) than for shoot parts (0.0002 to 0.0429) and used to obtain regression equations by time. Long-term BCFs estimated by the obtained equations ($R^2$ of 0.86 to 1.00) were evaluated with the maximum residue limit (0.1 mg/kg) of ED for radishes, in order to suggest safe management guidelines of ED for radish-cultivating soils. CONCLUSION: Suggested guidelines showed the significant dependency on duration for radish cultivation and exposed concentration of ED in soil.

• Korean Journal of Environmental Agriculture
• /
• v.36 no.1
• /
• pp.57-62
• /
• 2017

BACKGROUND: Pesticide residue analysis is essentially required for safety evaluation of agricultural products. Bistrifluron and chlorantraniliprole have been currently considered as potentials to deeply evaluate their residues in agricultural products because they are frequently found in strawberry. This work was performed to investigate the residual patterns of bistrifluron and chlorantraniliprole in strawberry after harvest. METHODS AND RESULTS: Strawberry was treated with bistrifluron and chlorantraniliprole 0, 1, 2, 3, 5, 7 and 10 days before harvest under greenhouse conditions. The strawberry samples were subjected to solvent and solid phase extractions followed by LC-MS/MS analysis. There covery percentages of bistrifluron and chlorantraniliprole for tified in the control samples ranged from approximately 82 to 103% with the method limit of 0.005 mg/kg. The concentrations of bistrifluron and chlorantraniliprole in strawberry samples decreased significantly in 10 days after treatment, giving the safety levels of 0.04 to 0.06 mg/kg at 10 days after application, as considered maximum residue limit. The half-lives of bistrifluron and chlorantraniliprole based on first order kinetics were determined to 6.3 days and 6.4 days, respectively. CONCLUSION: Bistrifluron and chlorantraniliprole are suggested to use in strawberry 10 days before harvest to reach residual safety levels.

• Korean Journal of Environmental Agriculture
• /
• v.36 no.1
• /
• pp.43-49
• /
• 2017

BACKGROUND: Greenhouse crops are one of agricultural products consumed largely in Korea. Cucumber is a typical example as main vegetables of greenhouse crops. Thus, pesticide residue analysis is an important requirement to guarantee pesticide safety of cucumber. This work was aim to investigate the residues of penthiopyrad and pyriofenone in cucumber after harvest. METHODS AND RESULTS: Cucumber was subjected to treat with penthiopyrad and pyriofenone at a level of recommended dose 0, 1, 2, 3, 5, 7 and 10 days before harvest under greenhouse conditions. The samples were extracted with organic solvent by using a homogenizer and purified on solid phase cartridge column followed by LC-MS/MS analysis. The recovery levels of penthiopyrad and pyriofenoneranged from approximately 81 to 93% with the method limit of 0.005 mg/kg and coefficient of variation less than 10%. Penthiopyrad and pyriofenone were detected at a level less than maximum residue limit in cucumber at 10 days before. The half-lives of penthiopyrad and pyriofenone were determined to 2.4 ~ 2.6 days. CONCLUSION: Penthiopyrad and pyriofenone are suggested to use in cucumber 10 days before harvest to reach their levels less than maximum residue limit.

• Journal of Food Hygiene and Safety
• /
• v.32 no.4
• /
• pp.298-305
• /
• 2017

Benzovindiflupyr is a new pyrazole carboxamide fungicide that inhibits succinate dehydrogenase of mitochondrial respiratory chain. This study was carried out to develop an analytical method for the determination of benzovindiflupyr residues in agricultural commodities using LC-MS/MS. The benzovindiflupyr residues in samples were extracted by using acetonitrile, partitioned with dichloromethane, and then purified with silica solid phase extraction (SPE) cartridge. Correlation coefficient ($r^2$) of benzovindiflupyr standard solution was 0.99 over the calibration ranges ($0.001{\sim}0.5{\mu}g/mL$). Recovery tests were conducted on 5 representative agricultural commodities (mandarin, green pepper, potato, soybean, and hulled rice) to validate the analytical method. The recoveries ranged from 79.3% to 110.0% and then relative standard deviation (RSD) was less than 9.1%. Also the limit of detection (LOD) and limit of quantification (LOQ) were 0.0005 and 0.005 mg/kg, respectively. The recoveries of interlaboratory validation ranged from 83.4% to 117.3% and the coefficient of variation (CV) was 9.0%. All results were followed with Codex guideline (CAC/GL 40) and Ministry of Food and Safety guideline (MFDS, 2016). The proposed new analytical method proved to be accurate, effective, and sensitive for benzovindiflupyr determination and would be used as an official analytical method.

• The Korean Journal of Pesticide Science
• /
• v.15 no.4
• /
• pp.335-349
• /
• 2011

100 residual pesticides in 1,565 medicinal herbs being on sale in Seoul was analyzed by a simultaneous multiresidue method. The recovery ratio was 71.0~119.7%. The detection rate of pesticide residues was 5.3% and the rate of excess to Maximum Residue Limits (MRLs) was 0.9% of the total samples. The medicinal herbs which had the high detection rate of residual pesticides were Alismatis Rhizoma, Citri Unshii Pericarpium, Lycii Fructus and Zyzyphi Fructus. The medicinal herbs detected pesticide over Maximum Residue Limits (MRLs) were Alismatis Rhizoma (4), Cnidii Rhizomain (4), Chrysanthemi Zawadski Herba (1), Citri Unshii Pericarpium (1), Lycii Radix Cortex (1), Menthae Herba (1), Schisandrae Fructus (1) and Taraxaci Herba (1). The residual pesticides which had the high detection frequency were cypermethrin, chlorpyrifos, phenthoate, endosulfan, isoprothiolane, chlorothalonil and chlorfenapyr. Estimated Daily Intake (EDI) of detected pesticides was compared to Acceptable Daily Intake (ADI) in order to assess risk. Ethoprophos detected in Cnidii Rhizomain showed the highest %ADI, 26.85. And pyraclofos and endosulfan in Cnidii Rhizomain, endosulfan and isoprothiolane in Alismatis Rhizoma and cyprodinil in Taraxaci Herba showed more than 1 %ADI, but others showed below 1 %ADI.

• The Korean Journal of Pesticide Science
• /
• v.18 no.3
• /
• pp.123-129
• /
• 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
• /
• v.19 no.1
• /
• pp.5-13
• /
• 2015

A chromatographic method for the determination of imazapyr, a non-selective herbicide, in agricultural commodities was developed to use safety control of pesticide residue on crops, and was fully validated as an official method for residue analysis. Agricultural commodities, mandarin (fruit), hulled rice (cereal grains), pepper (vegetables), potato (potatoes) and soybean (beans) were extracted with methanol and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2.5 by 4N hydrochloric acid. Finally, they were analyzed by high performance liquid chromatography coupled to UV detector (HPLC-UVD). The developed method had the linearity in the range of test concentrations with coefficients of determination ($r^2$) more than 0.99. Recovery studies were carried out at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. Recoveries were ranged between 72.1 to 108.0%, with relative standard deviations less than 10%. A consistent recovery was determined according to the CODEX guidelines (CAC/GL40, 2003). Finally, LC/MS with selected ion monitoring was also applied to confirm the suspected residues of imazapyr in agricultural samples. This developed method for determination of imazapyr residues in agricultural commodities. can be used as an official method.

• Journal of Food Hygiene and Safety
• /
• v.30 no.3
• /
• pp.272-280
• /
• 2015

A simultaneous official method was developed for the determination of phorate and its metabolites (phorate sulfoxide, phorate sulfone, phorate oxon, phorate oxon sulfoxide, phorate oxon sulfone) in livestock samples. The analytes were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Phorate and its metabolites were extracted from beef and milk samples with acidified acetonitrile (containing 1% acetic acid) and partitioned with anhydrous magnesium sulfate. Then, the extract was purified through primary secondary amine (PSA) and C18 dispersive sorbent. Matrix matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/L) for all the analytes into blank extract with $r^2$ > 0.996. For validation purposes, recovery studies were carried out at three different concentration levels (beef 0.004, 0.04 and 0.2 mg/kg; milk 0.008, 0.04 and 0.2 mg/kg, n = 5). The recoveries were within 79.2-113.9% with relative standard deviations (RSDs) less than 19.2% for all analytes. All values were consistent with the criteria ranges requested in the Codex guidelines. The limit of quantification was quite lower than the maximum residue limit (MRL) set by the Ministry of Food and Drug Safety (0.05 mg/kg). The proposed analytical method was accurate, effective and sensitive for phorate and its metabolites determination and it will be used to as an official analytical method in Korea.

• Korean Journal of Environmental Agriculture
• /
• v.40 no.4
• /
• pp.353-358
• /
• 2021

BACKGROUND: Prochloraz has been widely used as an imidazole fungicide on fruits and vegetables in Korea. Analytical approaches to evaluate prochloraz residues in herbal medicine are required for their safety management. In this study, we developed a GC-ECD method for quantitative determination of prochloraz in Platycodi Radix. The metabolite 2,4,6-trichlorophenol (2,4,6-T) was used as a target compound to evaluate total prochloraz residues as it is categorized to a representative residue definition of prochloraz. All residues containing 2,4,6-T were converted to 2,4,6-T and subjected to GC-ECD. METHODS AND RESULTS: In order to verify the applicability, the method was optimized for determining prochloraz and it metabolite 2,4,6-T in Platycodi Radix. Prochloraz and its metabolite 2,4,6-T residuals were extracted using acetone. The extract was diluted with and partitioned directly into dichloromethane to remove polar co-extractives in the aqueous phase. The extract was decomposed to 2,4,6-T, and then the partitioned ion-associate was finally purified by optimized aminopropyl solid-phase extraction (SPE). The limits of quantitation of the method (MLOQs) were 0.04 mg/kg and 0.02 mg/kg, respectively for prochloraz and 2,4,6-T, considering the maximum residue level (MRL) of prochloraz as 0.05 mg/kg in Platycodi Radix. Recovery tests were carried out at two levels of concentration (MLOQ, 10 MLOQ) and resulted in good recoveries (82.1-89.7%). Good reproducibilities were obtained (coefficient of variation < 2.8%), and the linearities of calibration curves were reasonable (r² > 0.9986) in the range of 0.005-0.5 ㎍/mL. CONCLUSION(S): The method developed in this study was successfully validated to meet the guidelines required for quantitative determination of pesticides in herbal medicine. Thus, the method could be useful to monitor prochloraz institutionally in herbal medicine.