• The Korean Journal of Pesticide Science
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• v.20 no.2
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• pp.93-103
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• 2016

A simultaneous analytical method was developed for the determination of isoxaflutole and metabolite (diketonitrile) in agricultural commodities. Samples were extracted with 0.1% acetic acid in water/acetonitrile (2/8, v/v) and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2 by 1 N hydrochloric acid. The analytes were quantified and confirmed via 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 ($0.02-2.0{\mu}g/mL$) for all the analytes into blank extract with $r^2$ > 0.997. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries were ranged between 72.9 to 107.3%, with relative standard deviations (RSDs) less than 10% for all analytes. All values were consistent with the criteria ranges requested in the Codex guideline (CAC/GL40, 2003). Furthermore, inter-laboratory study was conducted to validate the method. The proposed analytical method was accurate, effective, and sensitive for isoxaflutole and diketonitrile determination in agricultural commodities.

• Korean Journal of Food Science and Technology
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• v.42 no.1
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• pp.8-13
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• 2010

Bisphenol A diglycidyl ether (BADGE) and bisphenol F diglycidyl ether (BFDGE) were obtained by a polymerization reaction of epichlorohydrin (ECH) with bisphenol A (BPA) or bisphenol F (BPF). These compounds are commonly used as monomers or additives such as a polymerization stabilizer and a hydrochloric acid scavenger of epoxy resin, polyvinyl chloride (PVC)-containing organosols and polyester lacquers, that are applied to the internal surface of most canned foods to impart chemical resistance. The unreacted BADGE, BFDGE and their reaction products migrating from epoxy resin, PVC-containing organosol and/or polyester lacquer-based food packaging materials into the foods have recently become an issue of great concern because of increased customer demand for safety. This study was conducted to develop a rapid and sensitive simultaneous analysis method based on HPLC/FLD and HPLC/APCI-mass and to evaluate the concentration of BADGE, BFDGE and their metabolites, BADGE $H_2O$, BADGE $2H_2O$, BADGE HCl, BADGE 2HCl, BADGE HCl $H_2O$, BFDGE $H_2O$, BFDGE $2H_2O$, BFDGE HCl, BFDGE 2HCl and BFDGE HCl $H_2O$ for 133 canned food samples. The method provided a linearity of 0.9997-0.9999, a limit of detection of $0.01-0.13\;{\mu}g/mL$, a limit of quantitation of $0.03-0.44\;{\mu}g/mL$ and a recovery (%) of 85.64-118.18. The number of samples containing BADGE, BFDGE or their metabolites were: 28/133 (21.1%), with levels of 0.400-0.888 mg/kg being observed for aqueous foods (19/133) and 0.093-0.506 mg/kg being observed for oily foods (9/133).

• The Korean Journal of Pesticide Science
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• v.19 no.1
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• pp.5-13
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• 2015

A chromatographic method for the determination of imazapyr, a non-selective herbicide, in agricultural commodities was developed to use safety control of pesticide residue on crops, and was fully validated as an official method for residue analysis. Agricultural commodities, mandarin (fruit), hulled rice (cereal grains), pepper (vegetables), potato (potatoes) and soybean (beans) were extracted with methanol and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2.5 by 4N hydrochloric acid. Finally, they were analyzed by high performance liquid chromatography coupled to UV detector (HPLC-UVD). The developed method had the linearity in the range of test concentrations with coefficients of determination ($r^2$) more than 0.99. Recovery studies were carried out at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. Recoveries were ranged between 72.1 to 108.0%, with relative standard deviations less than 10%. A consistent recovery was determined according to the CODEX guidelines (CAC/GL40, 2003). Finally, LC/MS with selected ion monitoring was also applied to confirm the suspected residues of imazapyr in agricultural samples. This developed method for determination of imazapyr residues in agricultural commodities. can be used as an official method.

• Applied Biological Chemistry
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• v.22 no.2
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• pp.109-122
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• 1979

Present study was carried out to reduce residual toxicity of BHC insecticides inherent in the organochlorine pesticides. For This end, r-isomer, the most potent insecticidal component among the BHC stereoisomers, was isolated and thus fortified by means of solvent precipitation. In parallel, 3-(2,4,5-trichlorophenyl)-1-methyl urea was prepared in good yield from technical BHC via 1,2,4-trichlorobenzene, 1,2,4,-trichloronitrobenzene, and 2,4,5-trichloroaniline. In addition, certain merit of the compound which make it possible to use as a herbicide is discussed. The results are summarized as follows; 1. Recrystallizing technical BHC from methanol-water binary solvent system, r-isomer was enriched to 49.7% at 95% recovery of r-isomer. 2. By partitioning technical BHC in 85% of methanolic solution into chloroform, r-isomer was fortified to 89.6% at 90.5% recovery of r-isomer. 3. Yield of 1,2,4-trichlorobenzene from technical BHC was greatly dependent upon concentration of alkalies and to less degree on the alkalies. 4. Surfactants, in particular cationic a quartenary ammonium salt, increased yield of 1,2,4-trichlorobenzene from technical BHC by alkaline hydrolysis. 5. Conversion of 1,2,4-trichlorobenzene to 2,4,5-trichloronitrobenzene was effected almost quantitatively utilizing $HNO_3-H_2SO_4$ nitrating agent at low temperature. 6. Yield of 91.4% was observed for the synthesis of 2,4,5-trichloroaniline by reducing 2,4,5-trichloronitrobenzene in the presence of iron turning and hydrochloric acid. 7. Overall yield based on BHC of 3-(2,4,5-trichlorophenyl)-1- methyl urea was 60.8%. 8. Inhibition effects, both germination and growth, 3-(2,4,5-trichlorophenyl)-1-methyl urea on several crops were found comparable to or more potent than those of $linuron{\circledR}\;and\;diuron{\circledR}$. In addition, it was also noted that susceptibility to the prepared compound depended upon the crops as well as specific part (shoots, roots) of the plant exposed to the chemicals.