• Korean Journal of Environmental Agriculture
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• v.39 no.2
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• pp.130-137
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• 2020

BACKGROUND: Mefentrifluconazole and triticonazole are the triazole fungicides. The maximum residue levels for agricultural products need to be set up. Therefore, development of the official analytical method for determination of mefentrifluconazole and triticonazole residues from agricultural crops was necessary due to safety management, and then a simultaneous analytical method was developed for the determination of mefentrifluconazole and triticonazole in agricultural crops. METHODS AND RESULTS: Samples were extracted using acetonitrile and purified using dispersive solid phase extraction, and then detected with liquid chromatograph-tandem mass spectrometry (LC-MS/MS). Matrix-matched calibration curves (0.0025-0.25 ㎍/mL) were linear into a sample extract with r²>0.99. For validation, the recovery test was carried out at three fortification levels (LOQ, 10 LOQ and 50 LOQ) from agricultural samples. The results for mefentrifluconazole and triticonazole ranged between 92.3 to 115.3% and 91.4 to 108.5%, respectively and RSD (relative standard deviation) values were also below 6.0%. Furthermore, inter-laboratory was conducted to validate the method. CONCLUSION: All values were corresponded with the criteria ranges requested by both the CODEX (CAC/GL 40-1993, 2003) and MFDS guidelines (2016). Therefore, the proposed method can be used as an official analytical method for determination of mefentrifluconazole and triticonazole (triazole fungicides) in the Republic of Korea.

• Korean Journal of Environmental Agriculture
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• v.34 no.2
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• pp.111-119
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• 2015

BACKGROUND: Ethychlozate (ECZ) is a plant growth regulator of synthetic auxin for agricultural commodities (ACs). Accurate and sensitive method to determine ECZ in diverse ACs on global official purpose is required to legal residue regulation. As the current official method is confined to the limited type of crops with poor validation, this study was conducted to improve and extend the ECZ method using high-performance liquid chromatography (HPLC) in all the registered crops with method verification. METHODS AND RESULTS: ECZ and its acidic metabolite (ECZA) were both extracted from acidified samples with acetone and briefly purified by dichloromethane partition. ECZ was hydrolyzed to form ECZA and the combined ECZA was finally purified by ion-associated partition including hexane-washing. The instrumental quantitation was performed using HPLC/ FLD under ion-suppression of ECZA with no interference by sample co-extractives. The average recoveries of intra- and inter-day experiment ranged from 82.0 to 105.2% and 81.7 to 102.8%, respectively. The repeatability and reproducibility for intra- and inter-day measurements expressed as a relative standard deviation was less than 8.7% and 7.4%, respectively. CONCLUSION: Established analytical method for ECZ residue in ACs was applicable to the nation-wide pesticide residues monitoring program with the acceptable level of sensitivity, repeatability and reproducibility.

• Korean Journal of Environmental Agriculture
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• v.12 no.3
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• pp.255-263
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• 1993

The demand of safety assessment for pesticide residues in foods is growing in Korea. In order to assess the actual dietary exposure toward pesticide residues, the problems in utilization of pesticide residue data were reviewed and optimization of food factors applicable to Korean population was conducted. The problems and current status in setting pesticide residue tolerance-domestic and foreign-in foods were also argued. The conclusion is summarized as follows: (1) Anticipated residue estimates(ARE) calculated from field trial residue data, the percentage of crop treated, and the effects of cooking or processing should be utilized for dietary exposure assessment in a real sense. (2) Average daily intake of total foods per person in Korea was 1,104g in 1970's and 1,240g in 1980's. Much variation was observed between the two decades by food commodities. (3) Pesticide residue tolerances in Korea have been established at relatively lower levels in comparison with FAO/WHO or western countries. More extensive studies and data accumulation as related to tolerance setting are called for in future for the sake of health protection and smooth interstate trade.

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

• Analytical Science and Technology
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• v.26 no.3
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• pp.174-181
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• 2013

Pyrifluquinazon is classified with a quinazoline insecticide that regulates food intake by controling the feeding behavior acting on the endocrine or nervous system of pests such as aphids and white fly. To keep safety on pyrifluquinazon residues in agricultural commodities a simple, accurate and rapid analytical method was developed and validated using high performance liquid chromatograph (HPLC-UVD). The pyrifluquinazon residues acidified with 1% formic acid in samples were extracted with acetonitrile and partitioned with hexane subsequently to dichloromethane then purified with silica solid phase extraction (SPE) cartridge. The purified samples were detected using HPLC-UVD. The method was validated using apple and pear spiked with pyrifluquinazon at 0.02, 0.05 and 0.1 mg/kg and hulled rice, pepper, soybean at 0.05 and 0.1 mg/kg. Average recoveries were 70.5~107.9% with relative standard deviation less than 10%. The result of recoveries and overall coefficient of variation of a laboratory results in Gwangju regional FDA and Daejeon regional FDA was followed with Codex guideline (CODEX CAC/GL 40). This method is appropriated at pyrifluquinazon residues determination and will be used as official method of analysis.

• Korean Journal Plant Pathology
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• v.10 no.4
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• pp.297-304
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• 1994

This study was carried out to develop bioassay for detection of pesticide residues in agricultural products by using the soil microbial isolates sensitive to pesticides. One hundred bacterial isolates and eighty five fungal isolates were obtained from soil and their sensitivity to 10 ppm of several pesticides was examined in vitro. Five bacterial isolates and three fungal isolates were found sensitive to organochloride fungicide and two fungal isolates sensitive to organocopper fungicide. Among these isolates, B46, B93 and F67 were tested to find out the difference in sensitivity according to the methods of fungicide treatment. All of the isolates were found sensitive to 10 ppm of organochloride fungicides mixed directly in PDA. But they were found insensitive to the fungicide mixed in PDA after filtering through membrane filter. In case of organocopper fungicide, the isolates were found sensitive only when it was treated in PDA. And their sensitivity showed difference among various kinds of organochloride fungicides. B46 and B93 were employed to check the possibility as the agent for detection of the pesticidal residues in twenty eight agricultural products including rice. It was found that all samples had not residues because the samples did not inhibit the growth of isolates. When organochloride fungicides were applied to the above products, it was possible to detect the residues in fruits and vegetables at the concentration of 10 ppm, but not in starch-rich grains. B46 and B93 were identified as Bacillus sp. according to their bacterial characteristics in culture.

• Journal of Food Hygiene and Safety
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• v.25 no.2
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• pp.106-117
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• 2010

This study was carried out to investigate the current status of pesticide residues in 3,988 agricultural products in the northern area of Seoul from January to December in 2009. 3,988 samples comprising 109 types of agricultural products were assessed via a multiresidue method to detect 272 pesticides. Pesticide residues were detected in 25.6% (1,021 of 3,988 samples), and the rate at which the detected residues violated the maximum residue levels (MRLs) of the Korean Food Code was 2.2% (89 of 3,988 samples). The agricultural products which exceeded their maximum residue limits were leek, ginseng, welsh onion, crown daisy and lettuce (leaf). Additionally, the most frequently detected pesticide that exceeded the regulation maximum was endosulfan, procymidone, tolclofos-methyl, iprodione and flutolanil.

• Korean Journal of Environmental Agriculture
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• v.41 no.4
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• pp.261-275
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• 2022

BACKGROUND: Prior to implementing a positive list system (PLS), there is a need to establish acceptable daily intake (ADI) and maximum residue limit (MRL) for veterinary drugs that have been approved a few decades ago in South Korea. On top of that, chronic dietary exposure assessment of veterinary drug residues should be performed to determine whether the use of these veterinary drugs would cause health concerns or not. METHODS AND RESULTS: To establish the ADI, the relevant toxicological data were collected from evaluation reports issued by international organizations. A slightly modified global estimate of chronic dietary exposure (GECDE) model was employed in the exposure assessment owing to the limited residual data. Therefore, only the ADI of ephedrine was established due to insufficient data for the other veterinary drugs. Thus, instead of ADI, the threshold of toxicological concern (TTC) value was used for the other drugs. Lastly, the hazard index (HI) was calculated, except for etizazole hydrochloride, due to the potential of mutagenicity. CONCLUSION(S): The HI values of ephedrine, menichlopholan, and anacolin were found to be as high as 6.4%, suggesting that chronic dietary exposure to the residues from these uses was unlikely to be a public health concern. Further research for exposure assessment of veterinary drug residues should be performed using up-todate Korean national health and nutrition examination survey (KNHANES) food consumption data. In addition, all relevant available data sources should be utilized for identifying the potentials of toxicity.

• Journal of Food Hygiene and Safety
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• v.31 no.5
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• pp.319-326
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• 2016

Colistin is a last resort antimicrobial agent against multi-drug resistant Gram-negative bacteria. This study was conducted to develop an analytical method to determine colistin in fish and shrimp. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with acidified 5% methanol (containing 0.5% formic acid). Then, solid phase extraction (SPE) was used for cleanup. Matrix-matched calibration curves were linear over the calibration ranges (0.05-1.2 mg/kg) for all the analytes into blank sample with $r^2$ > 0.99. All the values fulfilled the criteria requested by the Codex guidelines. Average recoveries ranged from 85.9% to 107.9%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was less than 15%. The limit of detection (LOD) was 0.02 mg/kg, and the limit of quantitation (LOQ) was 0.05 mg/kg. This improved method showed higher accuracy and acceptable sensitivity to meet the CAC guideline requirements and is applicable for the analysis of residual colistin (A+B) in fish and shrimp.

• Korean Journal of Environmental Agriculture
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• v.24 no.1
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• pp.45-55
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• 2005

This study was undertaken to find out necessary measures to improve the tolerance setting system of pesticide residues on food crops in Korea which is scientifically reasonable and harmonizable with international standards. Information on tolerance setting systems of pesticide residues by Codex Alimentarius Commission, Joint FAO/WHO Meeting of Experts on Pesticide Residues, USA, EU, Japan and Taiwan was collected and analyzed. On the basis of information in the above countries, necessary actions to be taken by the Korean regulatory authorities were recommended with respect to priority setting, maximum residue limits (MRLs) setting based on field residue data, group MRLs, minor crop problems, quantitation limit and dietary intake assessment.