• The Korean Journal of Pesticide Science
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• v.14 no.4
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• pp.371-380
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• 2010

This study was performed to develop a precise single residue analytical method of fungicide cyprodinil in representative crops for using as general residue analytical methods which could be applied to most of crops. Apple, mandarin, Korean cabbage and green pepper were selected as representative crops, and they were macerated, extracted with acetonitrile, concentrated and partitioned with n-hexane. Then the extracts were concentrated and cleaned-up through silica gel column with ethyl acetate:n-hexane (15:85, v/v) before concentration and analysis with HPLC. LOQ (limit of quantitation) of cyprodinil was 5 ng (S/N>10) and MQL (method qnantitation limit) was 0.05 mg/kg. Recoveries were measured at three fortification levels (MQL, 10MQL and 100MQL) on crop samples and ranged from 82.0 to 108.2% and coefficients of variation were less than 10% regardless of sample type.

• The Korean Journal of Pesticide Science
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• v.19 no.4
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• pp.345-353
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• 2015

The aim of this study is to develop residue analysis method for fenoxanil, a MBI (melanin biosynthesis inhibitor) propionamide fungicide, had mainly been used to control rice blast, and disease of other crops, fruits, and vegetables by using GLC/NPD and GC/MS. Extraction with acetone and partition with n-hexane/dichloromethane (80/20, v/v) were performed from hulled rice, soybean, Kimchi cabbage, green pepper, and apple, then column clean-up with florisil was applied. Mean recoveries were 82.2%-109.1% with less than 7.2% of coefficients of variation and limit of quantitation was set at the concentration of 0.04 mg/kg from the five agricultural products through the determination by GLC/NPD equipped with DB-5 capillary column and single laboratory validation. As a confirmatory method, GC/MS selected ion monitoring (SIM) was set from m/z 125.0, 188.9, and 293.0. Developed method is expected to apply the single residue analysis of fenoxanil in agricultural products.

• The Korean Journal of Pesticide Science
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• v.20 no.4
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• pp.341-348
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• 2016

Residual patterns of fungicides fludioxonil and metconazole applied 2 or 3 times on wheat were investigated with consideration for their distribution rates in each compartment of wheat. Wheat samples collected at harvesting day were divided into three compartments such as grain, hull and straw, and the pesticide residue analysis was individually carried out to such compartments of wheat. The analytical methods of fungicide residues in wheat were acceptable, with recoveries of 84.3 to 113.3% and correlation coefficients of 0.1 to 4.7%. Due to the systemic characteristics, the residual amounts of metconazole in the grain part of wheat were greater as 0.13~0.17 mg/kg than those amounts (0.01-0.03 mg/kg) for fludioxonil. To absolute residue amounts of the fungicides in one wheat plant, their distribution rates in each compartment of wheat were the highest in straws (68.5-70.7%), followed by hulls (29.0-31.0%) and grains (0.2-0.8%).

• The Korean Journal of Pesticide Science
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• v.13 no.4
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• pp.223-231
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• 2009

This study was performed to develop a precise single residue analytical method of fungicide fenhexamid in representative crops for general residue analytical method which could be applied to most of crops. Korean cabbage, mandarin, apple and green pepper were selected, macerated, extracted with acetone, concentrated and partitioned with dichloromethane. Then the extracts were concentrated and cleaned-up through Florisil column with ethyl acetate/0.1% acetic acid in hexane [15:85, (v/v)] before concentration and analysis with HPLC. LOQ (Limit of Quantitation) of fenhexamid was 1 ng (S/N>10) and MQL (Method Quantitative Limit) was 0.01 mg/kg. Recoveries were measured at two fortification levels (10 MQL and 50 MQL) on crop samples and ranged from 85.2% to 94.8% (mean recoveries) and coefficients of variation were <10% regardless of sample type.

• Journal of Food Hygiene and Safety
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• v.33 no.4
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• pp.296-305
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• 2018

Spiroxamine, one of fungicides, is used to control powdery mildew in various crops and black yellow sigatoka in bananas. The major strength of spiroxamine is to control powdery mildew in various crops and bananas yellow sigatoka in bananas. The compound has shown a high level of activity, good persistence and crop tolerance. Besides powdery mildew, good control of rust, net blotch and Rhynchosporium diseases been indicated in cereals, together with a complementary activity against Septoria diseases. In 2017, the maximum residue limit (MRL) of spiroxamine established in Korea. According to Ministry of ood and rug afety) regulations, spiroxamine residues defined only parent compound. Thus, a analytical method is needed to estimate the residue level of the parent compound. The objective of this study was to develop and validate analytical method for spiroxamine in representative agricultural commodities. Samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interfering substances. The analyte were quantified and confirmed liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive-ion mode using multiple reaction monitoring (MRM). Matrix matched calibration curves were linear over the calibration ranges ($0.0005{\sim}0.1{\mu}g/mL$) for the analyte in blank extract with coefficient of determination ($r^2$) > 0.99. For validation purposes, recovery studies will be carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries 70.6~104.6% with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges in the Codex guidelines (CAC/GL40, 2003) and MFDS guidelines. proposed analytical method be used as an official analytical method in the Republic of Korea.

• The Korean Journal of Pesticide Science
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• v.19 no.4
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• pp.424-427
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• 2015

Damping-off is a critical disease on ginseng seedling, which caused by the fungal pathogen Rhizoctonia solani. The disease has been prevented by tolclofos-methyl for the last 20 years. However, the tolclofos-methyl usually detected on the harvested roots of 6-year-old ginseng. Herein, we tried to select an alternative pesticide which not only must be safe but also efficiently inhibits the fungal pathogen. Four fungicides (fludioxonil, flutolanil, pencycuron, and thifluzamide) were applied to their inhibition efficacy against the pathogen. In in vitro test, fludioxonil treatment showed 80% inhibition activity for 25 days. Thifluzamide and flutolanil showed the activity for 10 days. Pencycuron showed for 1 days. In addition, the fludioxonil was more effective to control the pathogen comparing to other three fungicides in field. The incidence of damping-off was reduced to 71% by fludioxonil treatment. The level of the fungicide residue in seedling was 0.44 mg/kg, which value will be a negligible level in final products after 5 years. Consequently, the fludioxonil is a conceivable alternative for tolclofos-methyl to cope with R. solani.

• Journal of Applied Biological Chemistry
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• v.63 no.2
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• pp.153-159
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• 2020

The analytical method was established for simultaneous determination of fungicide prochloraz and its metabolites in several animal commodities using gas chromatography (GC) coupled with electron capture detector (ECD). Samples including beef meat, pork meat, chicken meat, milk, and egg were hydrolyzed with pyridine hydrochloride which converts prochloraz and its metabolites to 2,4,6-trichlorophenol (2,4,6-TCP) because residue definition for prochloraz was 'sum of prochloraz and its metabolites containing the 2,4,6-trichlorophenol moiety, expressed as prochloraz', for compliance with MRLs from animal commodities. Therefore, residual prochloraz was extracted with acetone, decomposed to 2,4,6-TCP, partitioned with dichloromethane, purified with aminopropyl SPE and quantified as 2,4,6-TCP with GC-ECD. The instrumental limit of quantitation and method LOQ (MLOQ) was 0.01 ㎍/mL and 0.02 mg/kg for prochloraz and 0.005 ㎍/mL and 0.01 mg/kg for 2,4,6-TCP, respectively. The linearity of the calibration curve was good with R² >0.995 in the range of 0.005-0.2 ㎍/mL. Fortification levels of prochloraz were 0.02 mg/kg (MLOQ) and 0.2 mg/kg (10MLOQ) for recovery tests. Overall recoveries of prochloraz were >90% with <10% of coefficient variation (C.V.). This established analytical method was fully validated and could be useful for quantification of prochloraz and its metabolites in animal commodities as official analytical method.

• 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.

• Journal of Life Science
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• v.33 no.10
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• pp.842-850
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• 2023

Pyrrolnitrin, pyrrolomycin, and pyoluteorin are functional halogenated phenylpyrrole derivatives (HPDs) derived from microorganisms with diverse antimicrobial activities. Pyrrolnitrin is a secondary metabolite produced from L-tryptophan through four-step reactions in Pseudomonas fluorescens, Burkholderia cepacia, Serratia plymuthica, etc. It is currently used for the treatment of superficial dermatophytic fungal infections, has high antagonistic activities against soil-borne and foliar fungal infections, and has many industrial applications. Since pyrrolnitrin is easily decomposed by light, it is difficult to widely use it outdoors. As an alternative, fludioxonil, a synthetically produced non-systemic surface fungicide that is structurally similar and has excellent light stability, has been commercialized for seed and foliar treatment of plants. However, due to its high toxicity to aquatic organisms and adverse effects in human cell lines, many countries have established maximum residue levels and strictly control its levels. Pyrrolomycin and pyoluteorin, which have antibiotic/antibiofilm activity against Gram-positive bacteria and high anti-oomycete activity against the plant pathogen Pythium ultimum, respectively, were isolated and identified from microorganisms. This review summarizes the biosynthesis and production of natural pyrrolnitrin derived from bacteria and the characteristics of synthetic fludioxonil and other natural phenylpyrrole derivatives among the HPDs. We expect that a plethora of highly effective, novel HPDs that are safe for humans and environments will be developed through the generation of an HPD library by microbial biosynthesis and chemical synthesis.

• Journal of Applied Biological Chemistry
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• v.60 no.4
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• pp.343-349
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• 2017

This study was conducted to investigate the residual level and the amount of transfer to lettuce grown in field condition treated with the 5-methyl-1,2,4-triazolo[3,4-b][1,3]benzothiazole (Azoxystrobin). The field trials on lettuce were carried out at two different green houses located in Gwangju (Field 1) and Yongin (Field 2). Soil and lettuce samples were collected at different days after soil treatment of azoxystrobin with two different concentrations, respectively. Average recoveries for azoxystrobin ranged from 86.9 to 113.6% from soil and lettuce with the variation coefficient of 0.1-4.6%. The initial concentrations of azoxystrobin in Gwangju soil were 9.20, 11.00 mg/kg and decreased to 1.36, 2.70 mg/kg at 43 DAT (days after treatment) in field 1, while 1.06, 2.23 mg/kg decreased to 0.20 and 0.67 mg/kg at 36 DAT in field 2, respectively. The half-lives of azoxystrobin were about 19.4 and 23.3 days for the low and high concentration of azoxystrobin treated soils in field 1 and 11.5 and 17.8 days in field 2 soils, respectively. Residue levels of azoxystrobin in lettuce were not detected in filed 1 and field 2 soils, respectively.