• Bulletin of the Korean Chemical Society
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• v.33 no.7
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• pp.2224-2228
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• 2012

This study describes the ability of capillary electrochromatography (CEC) for the determination of imidacloprid and carbendazim in tomato samples. A novel liquid crystal crown ether modified hybrid silica monolithic column was synthesized, characterized and developed as separation column for the first time. Baseline separation of imidacloprid and carbendazim could be achieved using a mobile phase containing 90% (v/v) 20 mmol/L phosphate buffer (pH 7.0) and 10% (v/v) acetonitrile. The matrix matched calibration curves were linear with correlation coefficient $r^2$ > 0.9998 in the range of 0.20-10.00 mg/L. The limits of detection for imidacloprid and carbendazim were 0.061 and 0.15 mg/kg, respectively, which were below the maximum residue limits established by the European Union as well as Codex Alimentarius. Average recoveries for imidacloprid and carbendazim varied from 101.6-108.0% with relative standard deviations lower than 6.3%. This method was applied to the analysis of tomatoes collected from local markets.

• The Korean Journal of Pesticide Science
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• v.19 no.4
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• pp.361-369
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• 2015

This study investigated residual characteristics of bistrifluron and fluopicolide in Korean cabbage, and suggested the pre-harvest residue limits (PHRLs) based on their dissipation patterns and biological half-lives. The pesticides were sprayed on Korean cabbage in two different region under greenhouse conditions at the recommended dose, respectively. The samples for residue analysis were harvested at 0 (2 hr), 1, 2, 4, 6, 8 and 10 days after treatment, and analyzed by HPLC after clean-up with Florisil SPE. The limit of quantification (LOQ) was $0.03mg\;kg^{-1}$ for bistrifluron and fluopicolide, and the recoveries ranged from 87.2-110.6% with below 5% of RSD. The biological half-lives of field I and field II were 3.9 and 4.2 days for bistrifluron and 4.9 and 4.2 days for fluopicolide, respectively. The PHRL of bistrifluron and fluopicolide were recommended as 3.83 and $3.23mg\;kg^{-1}$ for 10 days before harvest, respectively.

• The Korean Journal of Pesticide Science
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• v.13 no.1
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• pp.13-20
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• 2009

Two insecticides, commonly used for Chinese cabbage, etofenprox and methoxyfenozide, were subjected to a field residue trial to evaluate safeties of the residues at harvest. The pesticides were sprayed onto the crop at recommended and double doses 10 days before the prearranged harvest and then sampling was done at 0, 1, 2, 3, 5, 7, 10, and 12 days after spraying. The amounts of pesticides residues in the crop were analyzed by chromatographic methods. Limits of detection (LODs) of both etofenprox and methoxyfenozide were $0.01mg\;kg^{-1}$ and mean recoveries were $96.76{\pm}2.67$ (CV=2.76%) and $95.84{\pm}2.57%$(CV=2.69%) in case of etofenprox and $103.26{\pm}3.21$ (CV=3.11%) and $94.50{\pm}1.35%$(CV=1.43%) in case of methoxyfenozide, respectively. Biological half-lives of etofenprox and methoxyfenozide were 3.2 and 3.5 days at the recommended dose and 2.7 and 3.5 days at the double dose, respectively. Initial residue levels of the pesticides at the recommended and double doses exceeded their MRLs, but final residue levels of the pesticides in the crop samples at harvest were less than their MRLs. The ratios of the EDI to ADI by intake the crop harvested 10 days after spraying were less than 4% of their ADIs, representing that residue levels of two pesticides at harvest were evaluated as safe.

• The Korean Journal of Pesticide Science
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• v.16 no.4
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• pp.308-314
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• 2012

In order to monitor the residual pesticides in environment friendly agricultural commodities, fruits and fruiting vegetables. Twenty-five agricultural commodities were collected twice in May and August 2011 from nine environment friendly agricultural commodities-selling supermarkets and retail stores located in eight major cities in Korea. The number of each agricultural commodity collected, 555 samples in total, was 152 organic agricultural products, 202 pesticide-free agricultural products and 201 low-pesticide agricultural products. Pesticide residues in samples were analyzed by multiresidue method for 245 pesticides using a GC-ECD/NPD and an HPLC-DAD/FLD and the peaks suspected as pesticides were identified with a GC/MSD. As a result of pesticide residue analysis, three pesticides, bifenthrin, EPN and chlorpyrifos, were detected from four samples including apple, representing a detection rate of 0.72%. The residue levels of the four pesticide-detected samples were less than their maximum residue limits (MRLs) but one pesticide EPN detected from pear exceeded its legible criterion of one twentieth MRL. Estimated daily intakes of the pesticides detected from fruits and fruiting vegetables were less than 0.76% of their maximum permissible intake.

• Korean Journal of Environmental Agriculture
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• v.30 no.4
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• pp.446-452
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• 2011

BACKGROUND: To investigate the dissipation patterns of 3 pesticides, azoxystrobin, difenoconazole and iprodione, on green garlic after field treatment pesticides were treated as foliar treatment by single application at recommended and double the recommended rates. METHODS AND RESULTS: Residue samples were harvested at 0, 1, 2, 5, 7 and 10 days post-treatment for azoxystrobin and 0, 1, 2, 5, 7, 10, 15 and 21 days post-treatment for difenoconazole and iprodione. After preparation the fortified samples were extracted and analyzed by gas chromotography-electron capture detector (GC-ECD) to determine the residue levels. Recoveries ranged from 87 to 109% for azoxystrobin, difenoconazole and iprodione at two different levels. The limit of Quantification (LOQ) values were 0.002 mg/kg for azoxystrobin and difenoconazole and 0.01 mg/kg for iprodione. CONCLUSION(S): Half-lives of azoxystrobin, difenoconazole and iprodione in green garlic after treatment were 1.2, 3.8 and 3.2 days at recommended and 1.4, 3.3 and 3.2 at double the recommended rate, respectively. Residue level of azoxystrobin, difenoconazole and iprodione in green garlic were below the maximum residue limits (MRLs) at 0 day, 0 day and 5 days, respectively. Therefore, these pesticide were considered that residues was satisfied to the requirement of domestic trade related to the consumer safety.

• Korean Journal of Environmental Agriculture
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• v.42 no.1
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• pp.71-81
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• 2023

An accurate and easy-to-use analytical method for determining isocycloseram and its metabolites (SYN549431 and SYN548569) residue is necessary in various food matrixes. Additionally, this method should satisfy domestic and international guidelines (Ministry of Food and Drug Safety and Codex Alimentarius Commission CAC/GL 40). Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) was used to determine the isocycloseram and its metabolites residue in foods. To determine the residue and its metabolites, a sample was extracted with 20 mL of 0.1% formic acid in acetonitrile, 4 g magnesium sulfate anhydrous and 1 g sodium chloride and centrifuged (4,700 G, 10 min, 4℃). To remove the interferences and moisture, d-SPE cartridge was performed before LC-MS/MS analysis with C₁₈ column. To verify the method, a total of five agricultural commodities (hulled rice, potato, soybean, mandarin, and red pepper) were used as a representative group. The matrix-matched calibration curves were confirmed with coefficients of determination (R²) ≥ 0.99 at a calibration range of 0.001-0.05 mg/kg. The limits of detection and quantification were 0.003 and 0.01 mg/kg, respectively. Mean average recoveries were 71.5-109.8% and precision was less than 10% for all five samples. In addition, inter-laboratory validation testing revealed that average recovery was 75.4-107.0% and the coefficient of variation (CV) was below 19.4%. The method is suitable for MFDS, CODEX, and EU guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

• The Korean Journal of Pesticide Science
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• v.17 no.4
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• pp.307-313
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• 2013

This study was carried out to investigate the residual characteristics of fungicide azoxystrobin and difenoconazole in Prunus mume fruits, and establish pre-harvest residue limits (PHRL) based on dissipation and biological half-lives of fungicide residues. The fungicides were sprayed onto the crop at recommended dosage once and 3 times in 7 days interval, respectively. The samples were harvested at 0, 1, 2, 4, 6, 8, 10, 12 and 14 days after treatment. These residual pesticides were extracted with QuEChERS method, clean-up with $NH_2$ SPE cartridge, and residues were analyzed by HPLC/DAD and GLC/ECD, respectively. Method quantitative limits (MQL) of azoxystrobin were 0.03 mg $kg^{-1}$ and of difenoconazole were 0.006 mg $kg^{-1}$. Average recovery were $93.2{\pm}2.49%$, $85.5{\pm}1.97%$ for azoxystrobin at fortification levels at 0.3 and 1.5 mg $kg^{-1}$, and $100.8{\pm}6.74%$, $87.6{\pm}9.92%$ for difenoconazole at fortification levels at 0.06 and 0.3 mg $kg^{-1}$, respectively. The biological half-lives of azoxystrobin were 5.9 and 5.2 days at recommended dosage once and 3 times in 7 days interval, respectively. The biological half-lives of difenoconazole were 9.3 and 8.0 days at recommended dosage once and 3 times in 7 days interval, respectively. The PHRL of azoxystrobin and difenoconazole were recommended as 5.32 and 1.64 mg $kg^{-1}$ for 10 days before harvest, respectively.

• Journal of Food Hygiene and Safety
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• v.7 no.1
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• pp.23-28
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• 1992

전남지방의 주요 재배단제에서 채취한 총 16종의 복숭아들에 대한 농약 잔류량 조사하였으며, 이들 복숭아를 수세 및 탈피 그리고 저장하였을 때의 농약 잔류량의 변화를 고찰하고자 하였다. 총 24종의 조사대상 농약중 TPN(Chlotothalonil) 및 Diazinon 그리고 Fenitrothion만이 3지점의 시료에서 검출되었으며 그 잔류량은 보사부에서 설정한 잔류허용기준(Maximum Residue Limits : MRL)에 크게 미달되는 수준이었다. 그러나 이들 시료들을 수세 및 탈피하지 않고 분석한 결과 TPN의 우 MRL을 훨씬 초과한 양이 검출되었는데, Diazinon은 MRL에는 미치니 못하였지만 수세 및 탈피한 시료들보다 높은 수준으로 검출되었다. 수세에 의한 복숭아중의 잔류농약의 경감효과는 TPN의 경우 63.4~66.4% 이었으며 Diazinon은 거의100% 수준이었다. 한편 탈피에 의한 잔류농약의 경감효과는 TPN 및 Diazinon 모두에서 대부분 제거되어 수세에 의한 경감보다도 훨씬 우수하다는 것을 알 수 있었다. 시료를 2주간 저장한 후 복숭아를 수세나 탈피를 하지 않거나 수세만 하여도 TPN과 Diazinon이 대부분 제거되며, 탈피를 한 경우는 별로 차이가 없었다.

• Journal of Applied Biological Chemistry
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• v.42 no.4
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• pp.191-196
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• 1999

A multiresidue analytical method was developed for eight acaricides including benzoximate, clofentezine, fenazaquin, fenothiocarb, fenpyroximate, hexythiazox, pyridaben, and tebufenpyrad in four major fruits using high-performance liquid chromatography (HPLC). All the confounds were extracted with acetone from apple, pear, grape, and citrus samples. The extract was diluted with saline water, and n-heaxane partition was followed to recover the acaricides. Florisil column chromatography was employed to further purify the sample extract. HPLC with ultraviolet absorption detection, using an octadecylsilyl column under the isocratic mobile phase of acetonitrile/water mixture, was successfully applied to separate and quantitate all the compounds in the purified extract. Recoveries of the eight acaricides from for fortified samples ranged 86.4~97.0%. Relative standard deviations of the analytical method were all less than 10%. Detection limits of the method were in the range of 0.02~0.05 mg/kg. The proposed method was reproducible and sensitive enough to evaluate the terminal residue of the eight acaricides in the fruit harvest.

• The Korean Journal of Pesticide Science
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• v.17 no.1
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• pp.1-5
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• 2013

This study was conducted to the amount of pesticide residue in 21 different kinds of 100 commercial flowering teas. Multi-residue analyses of 203 pesticides was performed using the GC-ECD, GC-NPD, GC-MSD, and LC-MS/MS. Pesticide residues were detected in 4 samples (4%) of which 4 samples (4%) violated the maximum residue limits. 4 samples violating the limit were all imported teas. Pesticides detected were chlorpyrifos, flufenoxuron, lufenuron, pyrimethanil and methoxyfenozide. These results indicate the need of continuous monitoring of pesticide residue needs for safety of flowering teas.