• Korean Journal of Environmental Agriculture
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• v.30 no.1
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• pp.52-59
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• 2011

BACKGROUND: This study was performed to investigate pre-harvest residue limit (PHRL) in Chwinamul, to estimate biological half-life for residue of each pesticide. Chwinamul was sprayed with pesticides of standard and double application rate. Chlorfenapyr and fenarimol were sprayed once on Chwinamul at 10 days before harvest, and it was sampled 7 times and analysed the residual change of two pesticides. METHODS AND RESULTS: Chwinamul sample was extracted with acetonitrile and partitioned with dichloromethane, and pesticide residues were determined with GCECD. Method quantitation limit (MQL) of chlorfenapyr was 0.10 mg/kg and that of fenarimol was 0.02 mg/kg. Recoveries of chlorfenapyr at two fortification levels of 1.0 and 5.0 mg/kg were $94.2{\pm}$1.70 and $99.0{\pm}1.61%$, respectively. Recoveries of fenarimol at two fortification levels of 0.2 and 1.0 mg/kg were $92.1{\pm}2.14$ and $83.1{\pm}1.98%$, respectively. CONCLUSION(s): The biological half-lives of chlorfenapyr were about 3.5 days at standard application rate, and 3.4 days at double application rate. The biological half-lives of fenarimol were about 6.0 days at standard application rate, and 5.9 days at double application rate. The PHRLs of chlorfenapyr were recommended as 13.02 and 6.25 mg/kg for 10 and 5 days before harvest, respectively. And the PHRLs of fenarimol were recommended as 2.80 and 1.67 mg/kg for 10 and 5 days before harvest, respectively.

• The Korean Journal of Pesticide Science
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• v.17 no.1
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• pp.6-12
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• 2013

Methoxyfenozide and novaluron were sprayed with single and triple treatments separately on peach during cultivation period. Samples were collected over 14 days, 8 times in total (0, 2, 4, 6, 8, 10, 12, 14 days). Methoxyfenozide and novaluron were extracted with acetone and partitioned with dichloromethane, and analyzed by HPLC/DAD. Method Quantitation Limit (MQL) were both 0.005 mg/kg, average recoveries of methoxyfenozide at two fortification levels of 0.05 and 0.25 mg/kg were determined $92.7{\pm}2.9%$ and $102.8{\pm}3.1%$, and novaluron were $98.2{\pm}4.8%$ and $96.7{\pm}9.0%$, respectively. The biological half-life of methoxyfenozide was about 4.41 days at single treatment, and 4.24 days at triple treatments. The biological half-life of novaluron was about 14.81 days at single treatment, and 14.50 days at triple treatments. Dissipation of pesticides on peach was influenced by growth dilution effect. In case of application of methoxyfenozide and novaluron following guidelines on safe use of pesticides, the final residue level was predicted to be lower than Maximum Residue Limit (MRL).

• The Korean Journal of Pesticide Science
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• v.14 no.1
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• pp.37-48
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• 2010

The diacylhydrazine insecticides, methoxyfenozide, chromafenozide and tebufenozide are new-generation insecticides. These insecticides induce premature molting and cause the death of insects by mimicking their hormone. Also, these insecticides have already been widely used for vegetables planting in worldwide. Highperformance liquid chromatography (HPLC) is the most widely used procedure for determination of each compound residues in crops. However, simultaneous analysis method of these diacylhydrazine insecticides was not reported. The purpose of this study is to develop a simultaneous determination procedure of methoxyfenozide, chromafenozide and tebufenozide residue in crops using HPLC-UVD/MS method. These insecticide residues were extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, apple, pepper, and Chinese cabbage. The extract was diluted with saline water, and dichloromethane partition was followed to recover these insecticides from the aqueous phase. Florisil column chromatography was additionally employed for final cleanup of the extracts. The analytes were quantitated by HPLCUVD/MS, using a $C_{18}$ column. The crops were fortified with each insecticide at two levels per crop. Mean recoveries ranged from 89.0 to 104.8% in five representative agricultural commodities. The coefficients of variation were less than 3.9%. Quantitative limits of methoxyfenozide, chromafenozide and tebufenozide were 0.04 mg/kg in crop samples. A HPLC-UVD/MS with selected-ion monitoring was also provided to confirm the suspected residues. The proposed simultaneous analysis method was reproducible and sensitive enough to determine the residues of methoxyfenozide, chromafenozide and tebufenozide in agricultural commodities.

• Analytical Science and Technology
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• v.22 no.1
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• pp.44-50
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• 2009

In this study, the use of purge & trap GC-MS technique for determination of methylmercury in sediment samples was described. The method detection limit of the method was determined as 0.06 ng/g and the recovery of the method was $102{\pm}11.4%$, with precisions better than 11.2%. The method was validated by analysis of CRMs such as ERM CC580 (estuarine sediment) and IAEA 405 (sediment). Additionally, the performance of the method was tested on river sediment samples and the analytical results were compared with those of the GC-CVAFS, which has been widely used for methylmercury analysis.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.45 no.3
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• pp.217-224
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• 2019

Phthalates, endocrine disrupting chemicals, are similar in structure to sex hormones and mainly show reproductive toxicity and developmental toxicity. In this study, we analyzed 11 phthalates, including 3 kinds of phthalates prohibited in cosmetic use and 8 kinds of phthalates regulated in 'Common standards for children's products safety' and EU cosmetic regulation (EC No. 1223/2009). The phthalate analysis was optimized using GC-MS/MS. In analytical method validation, this method was satisfied in specificity, linearity, recovery rate, accuracy and MQL. Therefore, we used this method to analyze 82 products of Nail cosmetics & polish. Although six phthalates such as DBP, BBP, DEHP, DPP, DIBP and DIDP were detected at concentrations of $1.0{\sim}59.8{\mu}g/g$g, they were suitable to Korean cosmetic standards. DIBP and DBP were detected at concentration of $1.1{\sim}2.6{\mu}g/g$ in artificial nail, DBP and DEHP were $1.4{\sim}2.5{\mu}g/g$ in glue for nails, and DIBP, DBP, and DEHP were $2.5{\sim}33.3{\mu}g/g$ in nail stickers. Although substances such as DBP and DEHP in artificial nail, Glue for nails, and nail stickers were detected, they were suitable to 'Common safety standards for children's products. DIBP is not a regulated substance in Korea but showed the third highest detection rate following DBP (84.6%) and DEHP (63.4%). The concentration of phthalates detected in nail products is considered to be safe in current standards but continuous monitoring and research about non-regulated substances are also needed to be considered.

• Korean Journal of Food Science and Technology
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• v.51 no.4
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• pp.316-323
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• 2019

It is difficult to analyze pymetrozine in citrus fruits using the hydromatrix method because of its low efficiency of purification and overlap of matrix and pymetrozine peaks. Liquid-liquid extraction can analyze pymetrozine in citrus fruits using dichloromethane. Since low pH interferes with the extraction of pymetrozine, the extracts of citrus fruits were maintained over pH 7.0 by adding borax buffer and 1 N NaOH in the improved method. According to the improved method, citrus fruits (such as lemon, lime, orange, tangerine, and grapefruit) were extracted and purified for HPLC-photo diode array analysis. The results of validation were as follows: $4.360{\mu}g/kg$ of limit of detection, $14.533{\mu}g/kg$ of limit of quantitation, and 0.007 mg/kg of method quantitative limit. Citrus fruits spiked with pymetrozine showed a recovery range from 71.8 to 83.7% and a coefficient of variation below 6%. Thus, the improved method can efficiently analyze pymetrozine in citrus fruits.