• Korean Journal of Environmental Agriculture
• /
• v.30 no.2
• /
• pp.166-172
• /
• 2011

BACKGROUND: Food Sanitary Act establishes Maximum Residue Limits (MRLs) of pesticides in food that are newly registered and used per each quarter, as stipulated by Agro-chemical Control Act. Current Food Code contains the MRLs for a total of 418 pesticides in 184 food types. METHODS AND RESULTS: National MRLs for pesticides have been established by based on scientific data of good agricultural practice, acceptable daily intake (ADI), food intake, average body weight and others. MRLs for pesticides are generally set under the principle that theoretical maximum daily intake (TMDI) are always below ADI. As results, 27 MRLs in agricultural products were newly proposed for 22 pesticides (fungicide: azoxystrobin, fludioxonil, fluquinconazole, flusilazole, iprovalicarb, kresoxim-methyl, mandipropamid, metconazole, pyraclostrobin, tebuconazole, triflumizole, etc., Insecticide: dinotefuran, flubendiamide, indoxacarb, cyhalothrin, spinetoram, thiacloprid, thiamethoxam, metaflumizone, etc., Acaricide(miticide): cyenopyrafen, lufenuron) in 2010. CONCLUSION(s): There is no intake concerns for establishment of pesticide MRLs on foods in this time. Because the ratio of theoretical maximum daily intake (TMDI) are set below that of ADI.

• Journal of Food Hygiene and Safety
• /
• v.37 no.4
• /
• pp.238-248
• /
• 2022

This study was conducted to evaluate the safety of 208 types of residue pesticides on 150 dried agricultural products in Ulsan. The pesticide residues were detected using GC-MS/MS, LC-MS/MS, GC/ECD, GC/NPD, and LC/PDA. The detection rate was 19.3% (29 of 150 samples), and 28 types of pesticides were detected. Two of the 29 pesticide residues exceeded the maximum residue limit (MRL). Difenoconazole was detected in Ulleungdo aster, and chlorothalonil and chlorpyrifos were detected in chili pepper leaves. In the vegetable group, the frequency of pesticide residues was found to be the highest in dried leafy vegetables, followed by dried fruiting vegetables other than cucurbit vegetables, and then dried stalk and stem vegetables. The pesticide types detected in the commercial dried agricultural products were fungicide (60%), insecticide (23.8%), and acaricide (16.3%). In the validation study, the values of limit of detection (LOD), limit of quantitation (LOQ), coefficient of determination (R²), and recovery rate were in the range of 0.0001-0.0409 mg/kg, 0.0003-0.1241 mg/kg, 0.994-0.999, and 81.58-116.79%, respectively. The ratio of estimated daily intake (EDI)/acceptable daily intake (ADI) was 0.00002-0.31395%.

• Journal of Applied Biological Chemistry
• /
• v.52 no.3
• /
• pp.126-132
• /
• 2009

In order to elucidate the relationship between the rainfastness of fungicides and their water solubilities, the fungicide residues on the leaf surface of hot pepper was assessed and compared after the drop-wise applications of fungicide solutions on leaf surface followed by artificial raining. As the raining was progressed after application of aqueous acetone solution of fungicides, the residue levels of fungicides were drop rapid at the early stage of raining, but the decreasing rates of residue level were slowed down thereafter. The initial rainfastness was reversely proportional to the water solubilities of the fungicides. Whole amount of dimethomorph residue, which water solubility is 18 mg/L, was washed off by 2.5 mm of raining. Although WP formulations of fungicides showed remarkable decreases of rainfastness compared to the aqueous acetone formulations, the fungicides having low water solubility showed better rainfastness. Chlorothalonil and mepanipyrim suspension concentrates was better in rainfastness than their WP formulation, and the rainfastness of mepanipyrim suspension was reversely proportional to the median diameter of suspension particles in the range of 1 to 4 ${\mu}m$. In brief, the rainfastness of 5 fungicides tested on the pepper leaf was, in the early stage of raining, closely related to water solubility. But, as the raining is progressed, the effect of the unknown factor, which is related with the particle size of fungicides, becomes serious.

• Journal of Food Hygiene and Safety
• /
• v.34 no.2
• /
• pp.140-147
• /
• 2019

An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

• Korean Journal of Environmental Agriculture
• /
• v.40 no.2
• /
• pp.108-117
• /
• 2021

BACKGROUND: Dichlobentiazox is a newly registered pesticide in Korea as a triazole fungicide and requires establishment of an official analysis method for the safety management. Therefore, the aim of this study was to determine the residual analysis method of dichlobentiazox for the five representative agricultural products. METHODS AND RESULTS: Three QuEChERS methods were applied to establish the extraction method, and the EN method was finally selected through the recovery test. In addition, various adsorbent agents were applied to establish the clean-up method. As a result, it was found that the recovery of the tested pesticide was reduced when using the d-SPE method with PSA and GCB, but C₁₈ showed an excellent recovery. Therefore this method was established as the final analysis method. For the analysis, LC-MS/MS was used with consideration of the selectivity and sensitivity of the target pesticide and was operated in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 70-120%, with standard deviation and coefficient of variation of less than 3.0% and 11.6%, respectively. CONCLUSION: Dichlobentiazox could be analyzed with a modified QuEChERS method, and the method determined would be widely available to ensure the safety of residual pesticides in Korea.

• The Korean Journal of Pesticide Science
• /
• v.19 no.3
• /
• pp.185-194
• /
• 2015

This study was performed to establish a single residue analytical method for determining fungicide carpropamid residues in various agricultural commodities. Korean cabbage, apple, brown rice and green pepper were selected as representative crops. Samples were homogenized, extracted with acetone and purified by liquid-liquid partition and Florisil column chromatography. Carpropamid residues were analyzed at 220 nm with reversed phase HPLC equipped octylsilyl and octadecylsilyl column and confirmed using mass spectrometry. ILOQ (Instrumental limit of quantitation) of carpropamid was 2 ng and MLOQ (Method LOQ) was 0.02 mg/kg. Mean recoveries from four kinds of crop samples fortified at three levels (MLOQ, 10LOQ, 100LOQ) in triplicate were in the range of 84~112%. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types.

• Applied Biological Chemistry
• /
• v.25 no.2
• /
• pp.93-98
• /
• 1982

Residues of Fujione (Fudiolan, fungicide) and Ortran (Acephate, insecticide) in Korean rice crop were studied. Also the persistencies of the pesticides in rice paddy soil were investigated in field and in laboratory. The residual levels of the pesticides in rice plant, straw, unpolished and polished rice were varied with the application rates of the pesticides. The residues of Fujione and Ortran in unpolished rice were $0.07{\sim}0.09ppm$ and $0.01{\sim}0.53ppm$, respectively. The half life of Fujione was 30 days under aerobic and 150 days under flooded condition in the laboratory system. Whereas in the paddy field it was about 100 days. In the case of Ortran it was $3{\sim}4$ days and $13{\sim}14$ days in aerobic and flooded condition, respectively in laboratory system.

• The Korean Journal of Pesticide Science
• /
• v.8 no.3
• /
• pp.198-209
• /
• 2004

In order to elucidate the behavior of the fungicide hexaconazole in soil and rice plants, rice plants were grown for 42 days in a microecosystem (pot) containing fresh and 28 day-aged soil residues of $[^{14}C]$hexaconazole. The amount of $^{14}CO_2$ evolved during 28 days of aging was 0.11 % of total $^{14}C$-radioactivity treated and the averaged weekly degradation rate was 0.03%. Mineralization rates for 42 days of rice cultivation on fresh and aged paddy soils were 0.67% of the total $^{14}C$ in case of non-rice planting on aged soil and 1.17% in case of rice planting on aged soil, whereas 1.25% in non-rice planting on fresh soil and 1.72% in case of rice planting on fresh soil, suggesting that the amounts of $^{14}CO_2$ were evolved higher from fresh soils than aged ones and from rice-planting soils than non-planting ones. The amounts of volatiles collected were very low as background levels. Most of $^{14}C$-Radioactivity was remained in soil after 42 days of rice cultivation and $^{14}C$ absorbed through rice roots was distributed more in shoots than roots and translocated into the edge of shoots of rice plants. Amounts of non-extractable $^{14}C$ in soils were higher in rice planted soil than in non-planting soil. The distribution of non-extractable $^{14}C$ was increased in the order of humin>fulvic acid>humic acid. The amounts of $^{14}C$ translocated into rotational crop Chinese cabbage were 2.36 and 3.69% of the total $^{14}C$ in case of rice planted soil containing fresh and aged residues, respectively, suggesting that small amounts of $[^{14}C]$hexaconazole and its metabolite(s) were absorbed and their bound residues were more available than their fresh ones to Chinese cabbage.

• Korean Journal of Food Science and Technology
• /
• v.45 no.3
• /
• pp.285-292
• /
• 2013

This study was carried out to validate the safety of ametoctradin residues in agricultural commodities by developing an official analysis method. An analytical method was developed and validated using HPLC-PDA detectors. The samples were extracted with methanol, subsequently partitioned with dichloromethane and purified with florisil column chromatograph using acetone/hexane (30/70, v/v) as solvent. The method was validated by using grape, hulled rice, mandarin, and potato spiked with ametoctradin at 0.05 and 5.0 mg/kg, and pepper at 0.05 and 2.0 mg/kg. Average recoveries were 76-114.8% with relative standard deviation less than 10%, and the limit of detection and limit of quantification were 0.0125 and 0.05 mg/kg, respectively. The result of recoveries and overall coefficient of variation of the laboratory results from Gwangju regional Food and Drug Administration (FDA) and Daejeon regional FDA was accorded with Codex Alimentarius Commission Guideline (CAC/GL 40). Based on these results, this method was found to be appropriate for ametoctradin residue determination and can be used as the official method of analysis.

• Analytical Science and Technology
• /
• v.6 no.3
• /
• pp.283-288
• /
• 1993

The solvent extraction and clean up processes for the gas chromatographic determination of muarimol pesticide residues in apples were investigated and examined the changes of residual concentration with the passage of time. The extracted pesticide with methanol were partitioned with dichloromethane after adding sodium chloride solution. The separated solutions were concentrated and transfered to the alumina column for clean up, and eluated with 1-chlorobutane : methanol solution. As a results their recovering for 0.200 and 1.00ppm muarimol spiked on apples have shown 79~95%. Residual amounts of nuarimol in apple was 0.0830ppm when the fungicide was treated eight times until 3 days before its harvest. It seems to be safely used when nuarimol is treated six times until 7 days before harvest of apple.