• Analytical Science and Technology
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• v.22 no.6
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• pp.458-463
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• 2009

A new quantitative analytical method has been established for the rapid determination of flumethrin in honey products using high performance liquid chromatography (HPLC). Sample was dissolved and extracted in the mixture of water and acetonitrile (1:2). The extracts were purified with silica cartridge eluted by the mixture of hexane and dichloromethane (55:45) and analyzed at 266 nm using HPLC. The percentage recovery of flumethrin spiked in sample was found to be 90.2-97.8% and the limit of detection is 0.003 mg/kg. We validated the method for the linearity, the precision and the reproducibility. We investigated the residues of flumethrin in honey products retailed in market using the established method. Flumethrin was not detected at all among 130 samples of honey.

• Journal of Food Hygiene and Safety
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• v.31 no.6
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• pp.432-438
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• 2016

Ethoxyquin (EQ, 1,2-dihydro-6-ethoxy-2,2,4-trimethyl-quinoline) is quinoline-based antioxidant used in the animal feed and food industry to protect the raw materials and final products against oxidation. In recent years the use of synthetic antioxidants in fishmeal ingredients carry-over to farmed fish fillets has received increasing attention in food safety. This study was conducted to develop an analytical method to determine EQ in aquatic products. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with 1 N HCl (in case of flatfish extracted with 1 N HCl containing 10% acetonitrile). Then, solid phase extraction (SPE) was used for the cleanup. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.99, analyzed at 0.005-0.2 mg/kg concentration. The developed method was validated according to the Codex Alimentarius Commission (CAC) guideline. The limits of quantitation for EQ were 0.01 mg/kg. Average recoveries ranged from 81.3% to 107%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was below 10%. The analytical method was characterized with high accuracy and acceptable sensitivity to meet CODEX guideline requirements and would be applicable to analyze the EQ residue in aquatic products.

• Korean Journal of Environmental Agriculture
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• v.37 no.1
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• pp.57-65
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• 2018

BACKGROUND: An analytical method was developed using HPLC-UVD/MS to precisely determine the residue of flusulfamide, a benzenesulfonamide fungicide used to inhibit spore germination. METHODS AND RESULTS: Flusulfamide residue 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 large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives 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 an octadecylsilyl column in HPLC, flusulfamide was successfully separated from co-extractives of sample, and sensitively quantitated by ultraviolet absorption at 280 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop sample fortified with flusulfamide at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries ranged from 82.3 to 98.2% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of flusulfamide was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue.

• Korean Journal of Environmental Agriculture
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• v.34 no.4
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• pp.309-317
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• 2015

BACKGROUND: An analytical method was developed using GC-ECD/MS to precisely determine the residue of fipronil, a phenylpyrazole insecticide used to control a wide range of foliar and soil-borne pests.METHOD AND RESULTS: Fipronil residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and fipronil was partitioned into n-hexane/dichloromethane (20/80, v/v) to remove polar co-extractives in the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fipronil was separated and quantitated by GC-ECD using a DB-17 capillary column. Accuracy of the proposed method was validated by the recovery from crop samples fortified with fipronil at 3 levels per crop in each triplication.CONCLUSION: Mean recoveries ranged from 86.6% to 106.0% in five representative agricultural commodities. The coefficients of variation were less than 10%. Limit of quantitation of fipronil was 0.004 mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fipronil in agricultural commodities.

• 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.

• KDI Journal of Economic Policy
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• v.27 no.2
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• pp.155-203
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• 2005

This paper intends to provide information about whichgroups should receive particular attention from policies aimed at raising participation and employment. A detailed portrait of the diversity of non-employment is presented with description of the extent the under-represented groups stayed in situations of labor inactivity. Also, once in employment, how these groups move from one sector to another is a main interest in the analysis. Using longitudinal data (1998-2002) constructed from 'the economically active population survey', I followed individuals over a five-year period and analyzed how frequently inactive persons enter the labor market and how they change industries and statuses.

• Korean Journal of Food Science and Technology
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• v.43 no.2
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• pp.125-133
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• 2011

The purpose of this study was to develop a methodology to detect spinosad which are difficult to analyze by multi-component simultaneous analysis of pesticide residues. We monitored spinosad due to the paucity of related information. The spinosad was determined using HPLC with UV detector at 250 nm. Correlation coefficient ($r^2$) for standard curve of spinosad A and D at standard concentration of 0.1-5.0 mg/kg were 0.999, respectively. Limit of quantitation (LOQ) of HPLC analysis was 0.005 mg/kg while limit of detection (LOD) was 0.001 mg/kg. Recovery experiments were conducted on five representative agricultural products to validate the analytical method. The recovery of proposed methods ranged from 74.9% to 104.0% and relative standard deviations were less than 10%. Spinosad residues were investigated in 16 commodities collected from 22 provinces. In this study, residues on all samples were not detected.

• The Korean Journal of Pesticide Science
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• v.2 no.3
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• pp.90-95
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• 1998

Soil residues of paraquat (1,1-dimethyl-4,4-dipyridinium dichloride) were determined in apple, pear, grape, and peach orchards for which 15 sites each were selected randomly from the corresponding large-scale production area throughout the country. Strong adsorption capacity measured using wheat bioassay (paraquat concentration required to reduce 50% root growth of wheat, SAC-WB) was also investigated on the orchard soils and the paraquat residue level was calculated against total SAC-WB values (SAC-WB value + paraquat residue). Average bound residue of paraquat on the 60 sites was 6.9 ppm, while paraquat residue in apple orchard reached 20.2 ppm which was the highest among the orchards and was almost double as compared with those in the other three orchards. Loosely bound residue of paraquat determined on the bound residue high top five soils occurred less than 0.5 ppm detection limit. Average SAC-WB value was 276.1 ppm and there were no any correlations between the SAC-WB value and clay content, organic matter content, and cation exchange capacity of the orchard soils. Paraquat residue level of the orchard soils against total SAC-WB recorded 2.43%.

• The Korean Journal of Pesticide Science
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• v.17 no.1
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• pp.65-71
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• 2013

The modified QuEChERS method was evaluated for rapid determination of pesticide residues in spinach by gas chromatography-nitrogen phosphorous detector (NPD) and electron capture detector (ECD). Fifty GC-amenable pesticides which were most frequently detected in monitoring were selected in the current study. Matrix-matched calibration was performed. The detector response for all pesticides was linear with determination coefficients higher than 0.995. LODs for most compounds ranged between 0.001 and 0.1 ug/g, and about 90% of the compounds had LODs of less than 0.05 ug/g. LOQs ranged from 0.001 to 0.32 ug/g, which were well below the MRLs permitted for most of pesticides. In the majority of cases, the recoveries (80-120%) and relative standard deviations (RSDs) (less than 20%) were within acceptable levels except for dichlorvos, propamocarb, chlorothalonil, dichlofluanid, cyhalothrin and fenvalerate. Also, this method which is applied to routine samples showed good results when comparing with traditional multi-residue method.

• Korean Journal of Food Science and Technology
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• v.48 no.4
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• pp.317-322
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• 2016

A pesticide mix solution containing difenoconazole, lambda-cyhalothrin, and lufenuron was applied 3 times on field grown chili pepper at a fivefold overdose dilution concentration of the spray solution at a pre-harvest interval of 7 day. Difenoconazole, lambda-cyhalothrin, and lufenuron were detected at 4.43, 0.334, and 1.56 mg/kg, respectively, in raw chili pepper. Washing with water reduced the residue levels to 91.4, 94.3, and 85.3%, respectively. In dried chili pepper, the residues of difenoconazole, lambda-cyhalothrin, and lufenuron were 22.2 mg/kg (processing factor, Pf =5.01), 1.65 mg/kg (Pf =4.94), and 6.54 mg/kg (Pf =4.19). In the seeds, difenoconazole and lambda-cyhalothrin were not detected, and lufenuron was detected at 0.0075 mg/kg (n=1) and <0.005 mg/kg (n=2). Thus the pesticide residues in the seeds was negligible. In the seed oil, difenoconazole and lufenuron residues were 0.0263 and 0.0295 mg/kg, respectively (concentration factors=5.26 and 4.72). These concentration factors supported the theoretical concentration factor of 6.8, assuming that all of compound present in the seed are transferred into the oil.