• 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.

• Korean Journal of Weed Science
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• v.14 no.4
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• pp.298-313
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• 1994

Residue of herbicide napropamide [N,N-dimethyl-2-(1-napthoxy)-propionamide] and change of micro-organism were investigated in upland soil under different environmental conditions. Half-lives of degradation were 28.3 days in the sterile soil and 14.6 days in the nonsterile soil, respectively. These results suggest that microorganism remarkably affected the decomposition of napropamide. Napropamide was rapidly degraded in order of 60% > 80% ${\geq}$ 40% soil moisture content of field water-holding capacity. Numbers of bacteria and total microbes in 60% moisture content was more than those in 40% moisture content. The more the napropamide degradation was rapid in lower soil pH. The total number of microorganism increased by lapse of time after treatment of napropamide at pH 5.5. The decomposition rate of napropamide was rapid in the order of $27^{\circ}C$ > $37^{\circ}C$ > $17^{\circ}C$. At $17^{\circ}C$ of soil temperature actinomycetes in napropamide treatment plot was more than these in nontreatment plot and also at $27^{\circ}C$ and $37^{\circ}C$ bacteria in napropamide treatment plot was more than those in nontreatment plot. Napropamide degradation was more rapid and number of microorganism was more abundant at the concentration of 10ppm than at that of 20ppm. The half-life of napropamide was longer in the clay loam soil than in the silty loam soil. The half times in laboratory test than in upland field. Numbers of microbes in the experiment under all the test environmental condition was not significantly different between treatment and nontreatment of napropamide.

• Proceedings of the Korean Society of Crop Science Conference
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• 2006.04a
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• pp.612-613
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• 2006

• Journal of the Korean Society of International Agriculture
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• v.30 no.4
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• pp.339-346
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• 2018

Cyanazine is a member of the triazine family of herbicides. Cyanazine is used as a pre- and post-emergence herbicide for the control of annual grasses and broadleaf weeds. This experiment was conducted to establish a determination method for cyanazine, as domestic unregistered pesticide, residue in major agricultural commodities using HPLC-DAD/MS. Cyanazine was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and partitioned to dichloromethane for remove polar extractive in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized florisil column chromatography. On a $C_{18}$ column in HPLC, cyanazine was successfully separated from co-extractives of sample, and sensitively quantitated by diode array detection at 220 nm. Accuracy and precision of the proposed method was validated by the recovery experiment on every major agricultural commodity samples fortified with cyanazine at 3 concentration levels per agricultural commodity in each triplication. Mean recoveries were ranged from 83.6 to 93.3% in five major representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation(LOQ) of cyanazine was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring(SIM) technique was also provided to clearly identify the suspected residue.

• Korean Journal of Environmental Agriculture
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• v.17 no.3
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• pp.239-245
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• 1998

To investigate the formation of bound residue with soil organic materials by oxidative coupling, nitroaromatics and their reduced metabolites, the insecticide parathion and the herbicide asulam were incubated with oxidoreductase, laccase or horseradish peroxidase, in the presence or absence of humic monomers. Most of aminotoluenes and amino-nitrophenols were completely transformed while most of nitrotoluenes and nitrophenols remained unchanged by a lactase or horseradish peroxidase in the presence or absence of humic monomers. Amino-nitrotoluenes were not transformed without humic monomers, but the addition of various humic monomers caused a considerable difference in the transformation of amino-nitrotoluenes by a lactase or horseradish peroxidase. Amino-nitrotoluenes were most transformed in the presence of catechol, syringaldehyde and protocatechuic acid. The insecticide parathion with nitro group and its metabolite were not mostly transformed in the presence or absence of humic monomers. The herbicide asulam with amino group remained unchanged without humic monomers as well, but the stimulating effect on the transformation of asulam was caused by the addition of catechol, syringaldehyde, protocatechuic acid or caffeic acid with a lactase.

• Bulletin of the Korean Chemical Society
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• v.28 no.6
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• pp.947-952
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• 2007

Mycobacterium tuberculosis is a pathogen responsible for 2-3 million deaths every year worldwide. The emergence of drug-resistant and multidrug-resistant tuberculosis has increased the need to identify new antituberculosis targets. Acetohydroxy acid synthase, (AHAS, EC 2.2.1.6), an enzyme involved in branched-chain amino acid synthesis, has recently been identified as a potential anti-tuberculosis target. To assist in the search for new inhibitors and “receptor-based” design of effective inhibitors of tubercular AHAS (TbAHAS), we constructed four different structural models of TbAHAS and used one of the models as a target for virtual screening of potential inhibitors. The quality of each model was assessed stereochemically by PROCHECK and found to be reliable. Up to 89% of the amino acid residues in the structural models were located in the most favored regions of the Ramachandran plot, which indicates that the conformation of each residue in the models is good. In the models, residues at the herbicide-binding site were highly conserved across 39 AHAS sequences. The binding mode of TbAHAS with a sulfonylurea herbicide was characterized by 32 hydrophobic interactions, the majority of which were contributed by residue Trp516. The model based on the highest resolution X-ray structure of yeast AHAS was used as the target for virtual screening of a chemical database containing 8300 molecules with a heterocyclic ring. We developed a short list of molecules that were predicted to bind with high scores to TbAHAS in a conformation similar to that of sulfonylurea derivatives. Five sulfonylurea herbicides that were calculated to efficiently bind TbAHAS were experimentally verified and found to inhibit enzyme activity at micromolar concentrations. The data suggest that this time-saving and costeffective computational approach can be used to discover new TbAHAS inhibitors. The list of chemicals studied in this work is supplied to facilitate independent experimental verification of the computational approach.

• The Korean Journal of Pesticide Science
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• v.15 no.2
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• pp.134-139
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• 2011

To investigate an amount of pesticide residue in rice paddy field soils and greenhouse soil, this monitoring was carried out pesticide detection frequency and concentrations collected samples from 150 rice paddy field soils and 152 greenhouse soils of nationwide in the year of 2007, and 2008, respectively. The detection limit of pesticides of this experiment were ranged 0.001~0.005 ppm. In 2007, One hundred fifty samples were collected from rice paddy field soils in April and monitored for 120 wide-used pesticides. A total of 11 pesticides were detected four fungicides, four insecticides and three herbicides in paddy field soils. The highest concentration levels of pesticide detected were 0.84 ppm as herbicide oxadiazon, 0.81 ppm as fungicide isoprothiolane and 0.50 ppm as insecticide buprofezin. The detection frequencies range were 0~19.3%, and the frequency was 2.7% as isoprothiolane and 19.3% as oxadiazon in paddy field soils. In 2008, One hundred fifty two samples were collected from greenhouse soils in April and monitored for 120 wide-used pesticides. A total of 29 pesticides were detected six fungicides, sixteen insecticides and seven herbicides in greenhouse soils. high concentration levels of pesticide detected levels were 5.09 ppm as insecticide chlorfenapyr, 2.57 ppm as fungicide chlorothalonil and 0.72 ppm as herbicide oxadiazon. The detection frequencies range were 0~38.8%, and high frequencies were 38.8% as insecticide endosulfan, 13.2% as oxadiazone, 10.5% as fungicide hexaconazole and 7.2% as isoprothiolane in greenhouse soils, Total endosulfan and oxadiazon were showed high detection frequency of 38.8% and 13.2%, respectively.

• Korean Journal of Environmental Agriculture
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• v.38 no.4
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• pp.321-331
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• 2019

BACKGROUND: Pinoxaden is the phenylpyrazoline herbicide developed by Syngenta Crop Protection, Inc. and marketed on 2006. The maximum residue levels for wheat and barley were set by import tolerance. Thus, Ministry of Food and Drug Safety (MFDS) official analytical method determining Pinoxaden residue was necessary in various food matrixes. Satisfaction of international guideline of CODEX (Codex Alimentarius Commission CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) are additional pre-requirements for analytical method. In this study, liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was investigated to analyze residue of Pinoxaden (M4), which is defined as pesticide residue in Korea, in foods. METHODS AND RESULTS: Pinoxaden (M4) was extracted followed by acid digestion (2hr reflux with 1N HCl) and pH adjusting (pH 4-5 with 3% ammonium solution). To remove oil, additional clean-up step with hexane saturated with acetonitrile was required to high oil contained sample before purification. HLB cartridge and nylon syringe filter were used for purification. Then, samples were analyzed by LC-MS/MS using reserve phase column C₁₈. Five agricultural group representative commodities (mandarin, potato, soybean, hulled rice, and red pepper) were used to verify the method in this study. The liner matrix-matched calibration curves were confirmed with coefficient of determination (r²) > 0.99 at calibration range 0.002-0.2 mg/kg. The limits of detection and quantitation were 0.004 and 0.01 mg/kg, respectively, which were suitable to apply Positive List System (PLS). Mean average accuracies of pinoxaden (M4) were shown to be 74.0-105.7%. The precision of pinoxaden and its metabolites were also shown less than 14.5% for all five samples. CONCLUSION: The method investigated in this study was suitable to CODEX (CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

• Korean Journal of Environmental Agriculture
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• v.32 no.2
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• pp.128-135
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• 2013

BACKGROUND: This study was performed to develop a single residue analytical method for new herbicide metazosulfuron in crops. METHODS AND RESULTS: Brown rice, apple, mandarin, Kimchi cabbage and soybean were selected as representative crops, and clean-up system, partition solvent and extraction solvent were optimized. Instrumental limit of quantitation (ILOQ), linearity of calibration curve and method limit of quantitation (MLOQ) were determined based on the chromatography and whole procedures. For recovery tests, brown rice, apple, mandarin, Kimchi cabbage and soybean samples were macerated and fortified with metazosulfuron standard solution at three levels (MLOQ, 10 MLOQ and 100 MLOQ). And then those were extracted with acetonitrile, concentrated, and partitioned with ethyl acetate. Then the extracts were concentrated again and cleaned-up through $NH_2$ (aminopropyl) SPE cartridge with acetone : dichloromethane (1% acetic acid) (20 : 80, v/v) before concentration and analysis with HPLC. CONCLUSION(S): ILOQ of metazosulfuron was 2 ng (S/N${\geq}$10) and good linearity was achieved between 0.05 and 12.5 mg/Kg of metazosulfuron standard solutions, with coefficients of determination of 0.9999. MLOQ was 0.02 mg/Kg. Good recoveries from 74.1 to 116.9% with coefficients of variation (C.V.) of less than 10% were obtained, regardless of sample type, which satisfies the criteria of Korea Food and Drug Administration (KFDA). Those results were reconfirmed with LC-MS (SIM). The method established in this study is simple, economic and efficient to be applied to most of crops as an official and general method for residue analysis of metazosulfuron.

• The Korean Journal of Pesticide Science
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• v.3 no.1
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• pp.66-77
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• 1999

In order to elucidate the fate of the residues of the bipyridylium herbicide paraquat in soil, maize plants were grown for 4 weeks on the specially-made pots filled with two different types of soils containing fresh and 6-week-aged residues of [$^{14}C$]paraquat, respectively. The mineralization of [$^{14}C$]paraquat to $^{14}CO_{2}$ during the aging period and the cultivation period of maize plants amounted to $0.13{\sim}0.18%$ and $0.02{\sim}0.17%$, respectively, of the original $^{14}C$ activities. At harvest the roots and shoots contained less than 0.1% and 0.01% of the originally applied $^{14}C$ activities, respectively, whereas the $^{14}C$ activities remaining in soil were more than 97% in both soils. The water extractability of the soil where maize plants were grown for 4 weeks was less than 1.2% of the original $^{14}C$ activities. Most of the non-extractable soil-bound residues of [$^{14}C$]paraquat were incorporated into the humin fraction. Soil pHs during the aging of soil B and after cultivation in all treatments increased. The distribution of the $^{14}C$ activities in subcellular particles of the maize plant roots was the highest in the residue fraction(incompletely homogenized tissue). Dehydrogenase activities increased after vegetation, regardless of soil aging.