• The Korean Journal of Pesticide Science
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• v.21 no.1
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• pp.68-74
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• 2017

An analytical method for detecting metamifop residue in paddy water, soil, and rice with high performance liquid chromatography (HPLC) was developed. Water was extracted with ethyl acetate before analyzing by HPLC. Soil residues were extracted with acetone under acidic condition and after purifying with $Extrelut^{(R)}$ NT, and silica SPE, the residue was analyzed by HPLC. For residue analysis in rice, the procedure involved extraction with acetone, purification with $Extrelut^{(R)}$ NT, partitioning between acetonitrile/hexane, purification with silica SPE cartridge, and analysis by HPLC. The limit of detection (LOD) was 1.0 ng, limit of quantitation (LOQ) was 3.0 ng, and method limit of quantitation (MLOQ) were 0.001 mg/L for paddy water, 0.01 mg/kg for rice and soil, respectively. Standard calibration curve shows linearity from 0.05 mg/kg to 5.0 mg/kg ($R^2=0.9999$). The recoveries in fortified paddy water were $91.3{\pm}3.5%$ (0.01 mg/L level) and $93.2{\pm}6.3%$ (0.05 mg/L level). The recoveries in fortified paddy soils were $92.5{\pm}4.0%$ (0.1 mg/kg level) and $92.7{\pm}4.0%$ (0.5 mg/kg level) in soil A, while, $102.3{\pm}4.4%$ (0.1 mg/kg level) and $98.9{\pm}7.9%$ (0.5 mg/kg level) in soil B, respectively. The recoveries in fortified rice were $93.0{\pm}6.9%$ (0.1 mg/kg level) and $85.0{\pm}3.5%$ (0.5 mg/kg level). This method was proved to be effective and can be used to determine the metamifop residue in paddy water, paddy soil, and rice.

• Korean Journal of Environmental Agriculture
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• v.33 no.4
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• pp.388-394
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• 2014

BACKGROUND: Aclonifen is used as a systemic and selective herbicide to control a wide spectrum broad-leaf weeds by inhibition carotenoid biosynthesis, and then its MRLs(Maximum Residue Limits) will be determined in onion and garlic. In this study, a new official method was developed for aclonifen determination in agricultural products to routinely inspect the violation of MRL as well as to evaluate the terminal residue level. METHODS AND RESULTS: Aclonifen was extracted from crop samples with acetone and the extract was partitioned with dichloromethane and then purified by silica solid phase extraction(SPE) cartridge. The purified samples were detected GC using an ECD detector. Limits of detection(LOD) was 0.001 mg/kg and quantification(LOQ) was 0.005 mg/kg, respectively. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n=5). The recoveries were ranged from 74.3 to 95.0% with relative standard deviations(RSDs) of less than 8%. All values were consistent with the criteria ranges requested in the Codex guidelines(CAC/GL 40). CONCLUSION: The proposed analytical method was accurate, effective and sensitive for aclonifen determination and it will be used to as an official method in Korea.

• The Korean Journal of Pesticide Science
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• v.2 no.3
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• pp.96-106
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• 1998

Rice plants were grown for 42 days in the specially made micro-ecosystem(pot) containing two different soils treated with fresh and 60-day-aged residues of [$^{14}C$]quinclorac, respectively, to elucidate the behaviour of the herbicide quinclorac residues in the soils. Amounts of $^{14}CO_{2}$ evolved from two soils treated with different residues with and without vegetation were all less than 2.2% of the total $^{14}C$, indicating that there was little microbial degradation of quinclorac in soil. $^{14}C$-Radioactivity absorbed and translocated into rice plants from soil A and B containing fresh quinclorac residues was 8.4 and 24.2%, respectively, of the originally applied $^{14}C$, while 5.5 and 17.7%, in aged residue soils. These results indicate that larger amounts of $^{14}C$ were absorbed by rice plants from soil B with less organic matter and clay than soil A, and the uptake of [$^{14}C$]quinclorac and its degradation products decreased with aging in soil. After 42 days of rice growing, 84.5 and 61.8% of the $^{14}C$ applied freshly to soil A and B, respectively, remained in soil, whereas, in the case of aged soils, 86.3 and 67.7% of the $^{14}C$ applied did. Meanwhile, without vegetation, more than 98.3% of the $^{14}C$ applied, in both fresh and aged residues, remained in soil, suggesting that quinclorac was relatively persistent chemically and microbiologically. Most of the non-extractable soil-bound residues of [$^{14}C$]quinclorac were incorporated into the organic matter and largely distributed in the fulvic acid portion.

• Analytical Science and Technology
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• v.26 no.2
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• pp.154-163
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• 2013

The maximum residue limits of pyrimisulfan is set as 0.05 mg/kg in rice in 2011, so very reliable and sensitive analytical method for pyrimisulfan residues is required for ensuring the food safety of pyrimisulfan residues in agricultural products. In this study, a rapid and sensitive analytical method was developed and validated using liquid chromatography electrospray ionization tandem mass spectrometry (LC-MS/MS) for the determination of herbicide pyrimisulfan residues in agricultural products. Average recoveries of pyrimisulfan ranged from 88.7 to 99.3% at the spiked level of 0.005 mg/kg and from 90.1 to 94.2% at the spiked level of 0.05 mg/kg, while the relative standard deviation was less than 10%. Linear range of pyrimisulfan was between 0.01~1.0 ${\mu}g/mL$ with the correlation coefficient ($r^2$) 0.999 and limit of quantification was 0.005 mg/kg. The results of method validation were satisfied Codex guideline. The results revealed that the developed and validated analytical method is possible for pyrimisulfan determination in agricultural product samples and will be used as an official analytical method.

• The Korean Journal of Pesticide Science
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• v.2 no.1
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• pp.59-64
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• 1998

In order to elucidate the leaching behaviour of the herbicide bentazon in soil, soil columns(5cm ID ${\times}$ 34 cm L) were packed with three different soils up to 30 cm height, followed by the treatment of [$^{14}C$]bentazon, and rice plants(Oryza sativa L.) were grown for 9 weeks on these columns, with the columns without growing rice plants as the control for comparison. The amounts of $^{14}C$ activities percolated were about 92% of the originally applied $^{14}C$ irrespective of the physicochemical properties of the soils in the absence of rice plants, whereas $21{\sim}50%$ of the originally applied $^{14}C$ was percolated in the presence of rice plants, suggesting that the amounts of $^{14}C$ leached decreased remarkably in rice-cultivating soils. Bentazon leached faster in soil with higher pH and with lower organic matter content in the presence of growing rice plants. The amounts of $^{14}CO_{2}$ evolved from the soil columns were less than 0.2% of the originally applied $^{14}C$. Smaller amounts of $^{14}C$ were translocated into shoots via roots in soils with higher organic matter content. $^{14}C$ activities distributed into the aqueous phase of the leachate collected from the soil columns increased with leaching period and by rice cultivation, whereas the physico-chemical properties of soils did not exhibit any effect. The amounts of soil-bound residues increased remarkably by cultivating rice plants.

• Korean Journal of Weed Science
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• v.30 no.1
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• pp.34-42
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• 2010

Competitive ability, allelopathy, made the common ragweed (Ambrosia artemisiifolia var. elatior ) one of the most dangerous weeds in Korea. The aim of this research was to evaluate the role of common ragweed as test species under laboratory bioassay and glasshouse conditions. Inhibition effect of the leaf extract was higher than that of stem and root parts extracts on germination and seedling growth of weeds. The 5% concentration of leaf extract of common ragweed inhibited the germination rate of Echinochloa crus-galli, Digitaria sanguinalis and Cyperus microiria by 68.3, 74.6 and 87.3%, respectively, as compared to the control. Generally, increasing incorporation concentration inhibited seedling growth of weeds. Incorporation of 5% common ragweed residue significantly reduced the plant length of E. crus-galli, D. sanguinalis and C. microiria by 48, 63 and 68%, respectively, as compared to the control. Also, the values of dry weight were 72, 78 and 71%, respectively. Contrarily, the emergence rate of soybean and corn was not affected by the incorporation of 5% concentration of common ragweed residue. However, the dry weight was inhibited by 37 and 28%, respectively. These results suggest that common ragweed had the ability to control some weed species using toxic compounds like natural herbicide.

• Korean Journal of Environmental Agriculture
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• v.39 no.3
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• pp.246-252
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• 2020

BACKGROUND: Pesticides are broadly used to control weeds and pests, and the residues remaining in crops are managed in accordance with the MRLs (maximum residue limits). Therefore, an analytical method is required to quantify the residues, and we conducted a series of analyses to select and validate the quick and simple analytical method for tolpyralate in five agricultural products using QuEChERS (quick, easy, cheap, effective, rugged and safe) method and LC-MS/MS (liquid chromatography-tandem mass spectrometry). METHODS AND RESULTS: The agricultural samples were extracted with acetonitrile followed by addition of anhydrous magnesium sulfate, sodium chloride, disodium hydrogencitrate sesquihydrate and trisodium citrate dihydrate. After shaking and centrifugation, purification was performed with d-SPE (dispersive-solid phase extraction) sorbents. To validate the optimized method, its selectivity, linearity, LOD (limit of detection), LOQ (limit of quantitation), accuracy, repeatability, and reproducibility from the inter-laboratory analyses were considered. LOQ of the analytical method was 0.01 mg/kg at five agricultural products and the linearity of matrix-matched calibration were good at seven concentration levels, from 0.0025 to 0.25 mg/L (R²≥0.9980). Mean recoveries at three spiking levels (n=5) were in the range of 85.2~112.4% with associated relative standard deviation values less than 6.2%, and the coefficient of variation between the two laboratories was also below 13%. All optimized results were validated according to the criteria ranges requested in the Codex Alimentarius Commission (CAC) and Ministry of Food and Drug Safety (MFDS) guidelines. CONCLUSION: In conclusion, we suggest that the selected and validated method could serve as a basic data for detecting tolpyralate residue in imported and domestic agricultural products.

• Korean Journal of Environmental Agriculture
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• v.40 no.4
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• pp.260-269
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• 2021

BACKGROUND: Diquat dibromide is a fast-acting nonselective herbicide and plant growth regulator. In this study, in order to understand the possibility of unintentional pesticide contamination in the following crops, the phytotoxicity and transition of diquat dibromide residue in soil into the following crops such as pepper, radish, lettuce and corn have been assessed through phytotoxicity trial and residual evaluation in the unintentional contamination of the higher residual diquat dibromide. METHODS AND RESULTS: The pepper, radish, lettuce and corn were cultivated in the sandy soil and loam soil where the 35 mg/kg and 90 mg/kg diquat dibromide were applied, respectively. Mild growth inhibition symptoms were observed in radish, lettuce and corn crops at the 90 mg/kg- diquat dibromide treatment on the 30 day of cultivation. Diquat dibromide was analyzed using liquid chromatography QTRAP (LC-MS/MS). The recovery rates of diquat dibromide from soil and crop were determined within range from 89.1 to 116.4% with relative standard deviation less than 14.7%. Diquat dibromide residues in soil were found to be 23.90-30.22 and 69.59-82.57 mg/kg from the 35 mg/kg and 90 mg/kg of diquat dibromide-treated soil, respectively after 30 days of crop cultivation. This result implicates that diquat dibromide did not convert to metabolites and remained mostly in the soil, even though it was partially decomposed during crop cultivation. In addition, the diquat dibromide in pepper and radish that were grown for 47 days, and lettuce and corn that were cultivated for 30 days were detected to be 0.01 mg/kg or less in the sandy loam and loam soil where the 90 mg/kg diquat dibromide was applied. CONCLUSION(S): Diquat dibromide did not cause severe phytotoxicity in the following crops as well as it did not uptake and distribute to the following crops, even though it was considered to be residual in the soil.

• Korean Journal of Microbiology
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• v.29 no.2
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• pp.130-135
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• 1991

The effects of a herbicide butachlor[2-chloro-2', 6'-diethyl-N-(butoxymethyl) acetanilide] on the growth of the purple non-sulfur bacteria were investigated. The butachlor inhibited the growth of all species tested by 18-51%, except Rhodospirillum rubrum at concentrations of M, which would be field capacity. The photosynthetic growth rate of the species in the presence of butachlor was influenced by the nitrogen source. Cultures supplied with (NH&S04 showed a somewhat higher growth rate than those fixing dinitrogen, but they were more susceptible to butachlor (26-51%). On the contrary, butachlor enhanced the growth rate of Rhodospirillum rubrum in nitrogen gas conditions. When the culture was performed in medium with butachlor as the carbon source, the cells of fixing dinitrogen showed a higher exhaustion of butachlor than those supplemented with (N&)2S04, which exhaustion was examined by a decrease of the major absorbance at 213 nm and 260 nm. The exhaustion of butachlor as the carbon source had relation with the growth of the cells. The alkalization of culture supplemented with nitrogen gas was found in the cells treated with butachlor or untreated. The butachlor affected the carotenoid region but bacteriochlorophyll remained unaffected.

• Plant Biotechnology Reports
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• v.4 no.4
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• pp.329-334
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• 2010

Multiple sequence alignments showed that the prolines at the 25th, 129th, 153rd, 242nd, 322nd, and 434th amino acids in 5-enolpyruvylshikimate-3-phosphate synthase (EPSPS) from Agrobacterium sp. strain CP4 are strongly conserved in various prokaryotic EPSPS proteins. Single point mutations of the conserved prolines to alanine (P25A, P153A, P242A, P322A, and P434A) were introduced in the CP4 EPSPS in order to investigate the importance of the conserved prolines for the enzyme properties. The point mutations caused decreases in substrate binding affinity and catalytic efficiency as well as the glyphosate resistance, in general. Especially, the 25th and 242nd prolines located in the polypeptide hinges connecting top and bottom domains of CP4 EPSPS as well as the 434th proline at the C-terminus of the enzyme turned out to be crucial for the enzyme activity.