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

• Korean Journal of Agricultural Science
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• v.7 no.1
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• pp.52-58
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• 1980

This study was conducted to detect copper which is considered in the soils of orchards, since copper fungicide has been applied to fruit trees. Soil samples taken from the fields of the chief producing districts of apple (Chungju, Yesan, Daegu), pear (Yangju, Bucheon, Seonghwan) and citrus (Seogypo in Jeju island) were analysed by an atomic absorption spectrophotometer. The results obtained were summarized as follows ; 1. In orchards of apple, the amount of copper of soils from Yesan, Chungju and Daegu were ranged 2.6-171.3ppm, 2.2-136.1ppm and 14.3-134.6ppm, respectively. Very little copper was detected from the soils in the field which has been cultivated for less than 20 years. About 100ppm and 130-170ppm of copper were detected in the field which has been cultivated for 30 years and for 50-60 years, respectively. Most of the copper was detected in the surface layer of soils (0-10cm), while very low content of copper was detected in the deeper layer of soils (10-20cm). 2. In orchards of pear, 20-30ppm of copper was detected from the surface of soils in the field which has been cultivated for more than 30 years and the highest level of copper, 36.8ppm, was detected from Yangju area. The amount of copper of soils from Yangju, Seonghwan and Bucheon were ranged 3.6-36.8ppm, 9.7-19.4ppm and 3.6-24.7ppm, respectively. 3. In orchards of citrus of Jeju island, only trace amount and 23-38ppm of copper were detected in the fields cultivated for 15 years and 20-30 years, respectively. The highest level of copper, 57ppm, was detected from the surface layer of soils in the field which has been cultivated for 35 years, but in most of the soil samples tested, only the natural background level of copper, about 20ppm, was detected. 4. The levels of copper residue in all the soil samples tested were lower than the tolerance level (125ppm of copper which is extracted in 0.1N-HCl solution), except those of copperr residue, 130-170ppm, that were detected from the orchards of apple which have been under cultivation for 50-60 years. Hence no problem for the farming could be speculated with the present concentration of copper analysed.

• Journal of Food Hygiene and Safety
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• v.36 no.3
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• pp.220-227
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• 2021

Fluoroimide is a fungicide and is also used as a pesticide for persimmons and potatoes. The established fluoroimide pesticide analysis method takes a long time to perform and uses benzene, a carcinogen. In addition, a lower limit of quantification is required due to enforcement of the Positive List System. Therefore, this study aimed to improve the analysis method for residual fluoroimide to resolve the problems associated with the current method. The analytical method was improved with reference to the increased stability of fluoroimide under acidic conditions. Fluoroimide was extracted under acidic conditions by hydrogen chloride (4 N) and acetic acid. MgSO₄ and NaCl were used with acetonitrile. C₁₈ (octadecylsilane) 500 mg and graphitized carbon black 40 mg were used in the purification process. The experiment was conducted with agricultural products (hulled rice, potato, soybean, mandarin, green pepper), and liquid chromatograph-tandem mass spectrometry was used for the instrumental analysis. Recovery of fluoroimide was 85.7-106.9% with relative standard deviations (RSDs) of less than 15.6%. This study reports an improved method for the analysis of fluoroimide that might contribute to safety by substituting the use of benzene, a harmful solvent. Furthermore, the use of QuEChERS increased the efficiency of the improved method. Finally, this research confirmed the precise limit of quantification and these results could be used to improve the analysis of other residual pesticides in agricultural products.

• Journal of Food Hygiene and Safety
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• v.29 no.3
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• pp.234-240
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• 2014

Fluxapyroxad is classified as carboxamide fungicide that inhibits succinate dehydrogenase in complex II of mitochondrial respiratory chain, which results in inhibition of mycelial growth within the fungus target species. This study was carried out to assure the safety of fluxapyroxad residues in agricultural products by developing an official analytical method. A new, reliable analytical method was developed and validated using High Performance liquid Chromatograph-UV/visible detector (HPLC-UVD) for the determination of fluxapyroxad residues. The fluxapyroxad residues in samples were extracted with acetonitrile, partitioned with dichloromethane, and then purified with silica solid phase extraction (SPE) cartridge. Correlation coefficient($R^2$) of fluxapyroxad standard solution was 0.9999. The method was validated using apple, pear, peanut, pepper, hulled rice, potato, and soybean spiked with fluxapyroxad at 0.05 and 0.5 mg/kg. Average recoveries were 80.6~114.0% with relative standard deviation less than 10%, and limit of detection (LOD) and limit of quantification (LOQ) were 0.01 and 0.05 mg/kg, respectively. All validation parameters were followed with Codex guideline (CAC/GL 40). LC-MS (Liquid Chromatograph-Mass Spectrometer) was also applied to confirm the analytical method. Base on these results, this method was found to be appropriate fluxapyroxad residue determination and can be used as the official method of analysis.

• Journal of Applied Biological Chemistry
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• v.55 no.4
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• pp.235-239
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• 2012

While cultivating crops, it is important to predict the biological half-lives of applied pesticides to ensure the safety of agricultural products. Dissipation patterns of the triazole fungicides, such as diniconazole and metconazole, during the cultivation of apple were established by utilizing the dissipation curve. As well as, the biological half-lives of the pesticides in apples were calculated using the residue amounts of them. The apples were harvested from 0 to 14 days after spraying diniconazole (WP) and metconazole (SC) at a recommended and three times of the recommended dose. Initial concentrations of diniconazole in apple were 0.09 and 0.15 mg/kg at a recommended and three times of the recommended dose, respectively, which were below MRL 1.0 mg/kg established by KFDA. The equations of biological half-life were $C_t=0.0811e^{-0.179x}$(half life: 3.9 days) and $C_t=0.1451e^{-0.148x}$ (half life: 4.7 days), respectively. In case of metconazole, initial concentrations in apple were 0.10 and 0.25 mg/kg, below MRL 1.0mg/kg, and biological half-life equations were $C_t=0.0857e^{-0.055x}$ (half life: 12.6 days) and $C_t=0.2304e^{-0.052x}$ (half life: 13.3 days), respectively. Therefore, when triazole fungicides were applied during the cultivation of apple, the biological half-life need to be calculated with the optimal equation model.

• The Korean Journal of Pesticide Science
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• v.3 no.2
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• pp.47-53
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• 1999

Photosensitizing activities of some photosensitizers (PS) for the artificial diminution of pesticide residues on horticultural crops were investigated. Five fungicides, iprodione, bitertanol, chlorothalonil, myclobutanil, and dichlofluanid were sprayed on apple and cucumber, followed by the application of each selected photosensitizer, and the samples were collected 0, 1, 3, 7, 15 days after the photosensitizer application and analyzed for the residual amounts. Of the 40 photosensitizers tested, six selected on the basis of the eliminating effect of pesticide residues were PS-1 (aromatic ketone), PS-2 (aromatic amine), PS-3 (quinone), PS-4 (inorganic compound), PS-5 (organic acid salt), and PS-6 (semiconductor photocatalyst). The residual amount of iprodione after 15 days of the application of PS-1 was 74% of that of the control. For bitertanol, the residual amount after 15 days of the application of PS-1 accounted for 78% of that of the control. The residual amounts of chlorothalonil after 1 day of the application of PS-1 and PS-2 accounted for 56 and 54% of those of the control, respectively. The residual amounts of iprodione on cucumber after 3 days of the application of the photosensitizers PS-1 and PS-2 were 44 and 67% of those of the untreated control, respectively. For myclobutanil, the residual amount after 15 days of the application of PS-6 accounted for 45% of that of the control. In case of dichlofluanid, the residual amount after 3 days of the application of PS-1 accounted for 44% of that of the control. Based on the results, PS-1 turned out to be the most promising photosensitizer for the accelerated photodegradation of the above fungicides on apple and cucumber.

• 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.