• Korean Journal of Environmental Agriculture
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• v.22 no.3
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• pp.227-232
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• 2003

This study was conducted to evaluate the terminal residue of a new fungicide, KNF 1002, in cucumber and pepper under greenhouse and field conditions. When a microemulsion formulation (20%) of KNF 1002 was applied once or twice during $1{\sim}7$ days before harvest, its terminal residue in cucumber ranged <$0.02{\sim}0.20\;mg/kg$ under greenhouse condition. In pepper, its figure recorded $0.31{\sim}0.79\;mg/kg$ and $0.11{\sim}0.28\;mg/kg$ under greenhouse and field conditions, respectively. Much higher level of terminal residues was observed in leaves than those in fruits in pepper, showing $7.38{\sim}25.20\;mg/kg$ and $0.11{\sim}1.99\;mg/kg$ under greenhouse and field conditions, respectively. Cultivation condition affected evidently the residue level in pepper harvests. Residual pattern of KNF 1002 seemed to be comparable to strobilurin fungicides currently used.

• Korean Journal of Environmental Agriculture
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• v.23 no.3
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• pp.142-147
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• 2004

Dissipation pattern of tebuconazole was evaluated by establishing application methods of the fungicide, paper-bagging of grape during growth and washing of grape after harvest. Application times increased from three to five resulted in high levels of residues in grape. Tebuconazole in grapes was present in different residual patterns with periods after final treatment ranging from 7 to 25 days. Significant differences in the residual patterns were also found when tebuconazole was treated during three different application periods, possibly due to meteorological condition and/or grape growth during each period. At the range from 2.5 g to 7.5 g of grape granules, residues were higher in small-sized grape than in big-sized grape and were mostly distributed on the peel of the grapes. Paper-bagging was a critical factor for reducing the fungicide residue on the peel. flesh of bagged and no-bagged grape had very low level of residues, 0.01 mg/kg and 0.05 mg/kg, respectively. Residues on grape was effectively eliminated with the washing methods suggested, a consecutive sinking-washing system Using of detergent solution during washing showed maximum residue reduction from grape. The washing methods showed effective action on the removal of lower content providing complete elimination, or almost, of the residues.

• The Korean Journal of Pesticide Science
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• v.15 no.2
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• pp.149-159
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• 2011

Bentazone is benzothiadiazole group herbicide, and used to foliage treatment. This herbicide have already been widely used for cereals and vegetables planting in worldwide. This experiment was conducted to establish a determination method for bentazone residue in crops using HPLC-UVD/MS. Bentazone residue was extracted with acetone (adjusted pH 1 with phosphoric acid) from representative samples of five raw products which comprised hulled rice, soybean, apple, green pepper, and Chinese cabbage. The extract was diluted with saline water, and dichloromethane partition was followed to recover bentazone from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The bentazone was quantitated by HPLC with UVD, using a YMC ODS AM 303 ($4.6{\times}250$ mm) column. The crops were fortified with bentazone at 3 levels per crop. Mean recovery ratio were ranged from 82.0% for a 0.2 mg/kg in apple to 97.9% for a 0.02 mg/kg in Chinese cabbage. The coefficients of variation were ranged from 0.5% for a 0.02 mg/kg in soybean to 9.7% for a 0.02 mg/kg in Chinese cabbage. Quantitative limit of bentazone was 0.02 mg/kg in representative five crop samples. A LC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of bentazone in agricultural commodities.

• Horticultural Science & Technology
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• v.34 no.1
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• pp.183-194
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• 2016

This experiment was conducted to establish an official determination method to measure fluazinam residue in horticultural crops for import and export using GC-ECD/MS. Fluazinam residue was extracted with acetone from fresh samples of four representative horticultural products, the vegetable crops green pepper and kimchi cabbage, and the fruit crops mandarin and apple. The acetone extract was diluted with saline water and n -hexane partitioning was used to recover fluazinam from the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fluazinam was separated and quantitated by GC with ECD using a DB-17 capillary column. The horticultural crops were fortified with three different concentrations of fluazinam. Mean recoveries ranged from 82.5% to 99.9% in the four crops. The coefficients of variation were less than 10.0%. The quantitative limit of fluazinam detection was $0.004mg{\cdot}kg^{-1}$ in the four crop samples. GC/MS with selected-ion monitoring was also used to confirm the suspected residue. This analytical method was reproducible and sensitive enough to measure the residue of fluazinam in horticultural commodities for import and export.

• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.22-29
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• 2019

Validamycin A is an aminoglycoside fungicide produced by Streptomyces hygroscopicus that inhibits trehalase. The purpose of this study was to develop a method for detecting validamycin A in agricultural samples to establish MRL values for use in Korea. The validamycin A residues in samples were extracted using methanol/water (50/50, v/v) and purified with a hydrophilic-lipophilic balance (HLB) cartridges. The analyte was quantified and confirmed by 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 (0.005~0.5 ng) into a blank extract with $R^2$ > 0.99. The limits of detection and quantification were 0.005 and 0.01 mg/kg, respectively. For validation validamycin A, recovery studies were carried out three different concentration levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) with five replicates at each level. The average recovery range was from 72.5~118.3%, with relative standard deviation (RSD) less than 10.3%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the NIFDS (National Institute of Food and Drug Safety) guideline (2016). Therefore, the proposed analytical method is accurate, effective and sensitive for validamycin A determination in agricultural commodities.

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

• Proceedings of the Korean Society of Propulsion Engineers Conference
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• 1999.10a
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• pp.11-11
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• 1999

Sach의 Boring out 측정방법은 튜브 또는 실린더 등의 축대칭 부품의 3차원 잔류 응력을 측정하는데 적용할 수 있다. 이 방법은 잔류응력이 층제거시 이완된 변형율로부터 결정된다는 원리에 근거하고 있다. 적용시 가정사항으로는 1) 잔류응력 분포가 축대칭이어야 하고 2) 응력 분포가 축방향을 따라 균일해야 한다는 것이다. 그러나 실제부품은 길이가 제한되어 있기 때문에 잔류응력 분포가 균일하다는 가정이 적용될 수 없다. 본 연구에서는 시편의 길이 대 외경 비를 변화시켰을 때 유한요소해석을 이용하여 층제거시 이완된 변형율로부터 계산된 측정값과 유한요소 해석값을 비교하여 이 측정방법의 적용한계와 타당성을 조사하였으며 얻어진 결론은 다음과 같다. Sach의 Boring out 측정방법을 적용하기 위해서는 부품의 외경 대 길이 비가 3이상일 경우 측정값과 해석값은 거의 일치하는 경향을 보이며 비가 증가할수록 측정오차가 줄어들 것으로 판단된다.

• Journal of Food Hygiene and Safety
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• v.37 no.3
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• pp.136-142
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• 2022

The research aims to develop a rapid and easy analytical method for methoprene using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A simple, highly sensitive, and specific analytical method for the determination of methoprene in livestock products (beef, pork, chicken, milk, eggs, and fat) was developed. Methoprene was effectively extracted with 1% acetic acid in acetonitrile and acetone (1:1), followed by the addition of anhydrous magnesium sulfate (MgSO₄) and anhydrous sodium acetate. Subsequently, the lipids in the livestock sample were extracted by freezing them at -20℃. The extracts were cleaned using MgSO₄, primary secondary amine (PSA), and octadecyl (C₁₈), which were then centrifuged to separate the supernatant. Nitrogen gas was used to evaporate the supernatant, which was then dissolved in methanol. The matrix-matched calibration curves were constructed using 8 levels (1, 2.5, 5, 10, 25, 50, 100, 150 ng/mL) and the coefficient of determination (R²) was above 0.9964. Average recoveries spiked at three levels (0.01, 0.1, and 0.5 mg/kg), and ranged from 79.5-105.1%, with relative standard deviations (RSDs) smaller than 14.2%, as required by the Codex guideline (CODEX CAC/GL 40). This study could be useful for residue safety management in livestock products.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.242-250
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• 2019

An analytical method was developed for the determination of fenquinotrione, a triketone herbicide, in agricultural products. Fenquinotrione was metabolized to KIH-3653-M-2 in plants. Analyte extraction was conducted using 2% formic acid in acetonitrile and cleaned up using a hydrophillic-lipophillic balance (HLB) cartridge. The limits of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. Matrix-matched calibration curves were linear over the calibration ranges ($0.001{\sim}0.1{\mu}g/mL$) into a blank extract with $r^2>0.99$. The recovery results for fenquinotrione and KIH-3653-M-2 ranged between 81.1 to 116.2% and 78.0 to 110.0% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$) with relative standard deviation (RSD) less than 4.6%. All values were corresponded with the criteria ranges requested in 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 fenquinotrione in the Republic of Korea.

• 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.