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Procedures in Establishing Residue Limits of Pesticides on Food Crops in Korea (한국에서 농산물중 농약잔류 허용기준의 설정절차)

  • Lee, Mi-Gyung;Hong, Moo-Gi;Park, Kun-Sang;Choi, Dong-Mi;Lim, Moo-Hyuk;Lee, Su-Rae
    • Korean Journal of Food Science and Technology
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    • v.37 no.4
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    • pp.685-694
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    • 2005
  • Korean practices in tolerance setting of pesticide residues on food crops were compiled with an effort to harmonize with international standards. Based on scientific data including historical background, limit setting protocols, adoption of ADI values, food factors, nation's body weights, and regulatory margins which are required for the setting of maximum residue limits, necessary measures to be taken by Korean regulatory authorities were proposed.

Procedures in Establishing Residue Limits of Pesticides on Food Crops in Codex Alimentarius Commission and Foreign Countries (국제기구 및 외국에서 농산물중 농약잔류 허용기준의 설정절차)

  • Lee, Mi-Gyung;Hong, Moo-Gi;Park, Kun-Sang;Choi, Dong-Mi;Lim, Moo-Hyuk;Lee, Su-Rae
    • Korean Journal of Environmental Agriculture
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    • v.24 no.1
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    • pp.45-55
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    • 2005
  • This study was undertaken to find out necessary measures to improve the tolerance setting system of pesticide residues on food crops in Korea which is scientifically reasonable and harmonizable with international standards. Information on tolerance setting systems of pesticide residues by Codex Alimentarius Commission, Joint FAO/WHO Meeting of Experts on Pesticide Residues, USA, EU, Japan and Taiwan was collected and analyzed. On the basis of information in the above countries, necessary actions to be taken by the Korean regulatory authorities were recommended with respect to priority setting, maximum residue limits (MRLs) setting based on field residue data, group MRLs, minor crop problems, quantitation limit and dietary intake assessment.

Study for Residue Analysis of Fluxametamid in Agricultural Commodities

  • Kim, Ji Young;Choi, Yoon Ju;Kim, Jong Soo;Kim, Do Hoon;Do, Jung Ah;Jung, Yong Hyun;Lee, Kang Bong;Kim, Hyochin
    • Korean Journal of Environmental Agriculture
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    • v.38 no.1
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    • pp.1-9
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    • 2019
  • BACKGROUND: Accurate and simple analytical method determining Fluxametamid residue was necessary in various food matrices. Additionally, fulfilment of the international guideline of Codex (Codex Alimentarius Commission CAC/GL 40) was required for the analytical method. In this study, we developed Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) method to determine the Fluxametamid residue in foods. METHODS AND RESULTS: Fluxametamid was extracted with acetonitrile, partitioned and concentrated with dichloromethane. To remove the interferences, silica SPE cartridge was used before LC-MS/MS (Liquid Chromatography-Tandem Mass Spectrometry) analysis with $C_{18}$ column. Five agricultural commodities (mandarin, potato, soybean, hulled rice, and red pepper) were used as a group representative to verify the method. The liner matrix-matched calibration curves were confirmed with coefficient of determination ($r^2$) greater than 0.99 at calibration range of 0.001-0.25 mg/kg. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. Mean average accuracies were shown to be 82.24-115.27%. The precision was also shown to be less than 10% for all five samples. CONCLUSION: The method investigated in this study was suitable to the Codex guideline for the residue analysis. Thus, this method can be useful for determining the residue in various food matrices as routine analysis.

Study for Residue Analysis of Pinoxaden in Agricultural Commodities

  • Kim, Ji Young;Yoon, Eun Kyung;Kim, Jong Soo;Seong, Nu Ri;Yun, Sang Soon;Jung, Yong Hyun;Oh, Jae Ho;Kim, Hyochin
    • 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.

Establishment of Korean Maximum Residue Limits for Pesticides in Foods (한국의 식품중 농약 잔류허용기준 설정)

  • Park, Kun-Sang;Im, Moo-Hyeog;Choi, Dong-Mi;Jeong, Ji-Yoon;Chang, Moon-Ik;Kwon, Kwang-Il;Hong, Moo-Ki;Lee, Chul-Won
    • The Korean Journal of Pesticide Science
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    • v.9 no.1
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    • pp.51-59
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    • 2005
  • Korean maximum residue limits (MRLs) for pesticides have been established based on scientific data of good agricultural practice, acceptable daily intake (ADI), food intake, average body weight and others. MRLs for pesticides are generally set under the principle that theoretical maximum daily intake (TMDI) are always below ADI. As results, 104 MRLs are going to be newly established for 24 pesticides and 102 MRLs are going to be added for 63 pesticides that have regulation already, Among new pesticides, ethaboxam and flupyrazofos are effective components that are first developed in Korea. In case of dithiocarbamates, MRLs are classified by 3 groups such as dimethyldithiocarbamates, ethylenebis (dithiocarbamate)s and propineb.

Determination of tetracycline antibiotics in food (식품 중 테트라싸이클린계 항생물질의 분석)

  • Park, Dongmi;Jeong, Jiyoon;Chang, Moonik;Im, Moohyeog;Park, Kunsang;Hong, Mooki
    • Analytical Science and Technology
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    • v.18 no.3
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    • pp.250-256
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    • 2005
  • A selective method of high performance liquid chromatography with UV detector has been applied to determine 4 tetracycline antibiotics in the animal food, simultaneously. The targets were chlortetracycline (CTC), doxycycline (DC), oxytetracycline (OTC), and tetracycline (TC) that are used routinely in veterinary medicine for prevention and control of disease. Food samples were beef, pork, chicken, milk, whole egg, flatfish (Limanda yokohamae), jacopever (Sebastes hubbsi), seabream (Chrysophrys major), eel (Anguilla japonica) and lobster (Hommarus americanus). After extracting food samples with 20% trichloroacetic acid and McIlvaine buffer, they were purified by a $C_18$ SPE cartridge with 0.01M methanolic oxalic acid solution. The concentrated residue was re-dissolved in methanol, filtered, cleaned up and analyzed on a $C_18$ column. The mobile phase was a mixture of 0.01M oxalic acid and acetonitrile with a gradient ratio from 85:15 to 60:40. The UV wavelength was 365 nm. The overall recoveries were ranged from 71% to 98% and the limit of detections were 0.022 for CTC, 0.012 for DC and OTC and 0.009 mg/kg for TC at signal/noise > 3, respectively. As results, CTC, DC and TC were not detected in all selected food samples, however, OTC was detected in meat and fishes. The determined level of OTC was 0.04 ppm for pork, 0.17 ppm for flatfish and 0.05 and 0.08 ppm for jacopever, that were within the Maximum Residue Limits (MRLs) in the food.

Prevalence of Antibiotic Residues and Antibiotic Resistance in Isolates of Chicken Meat in Korea

  • Lee, Hyo-Ju;Cho, Seung-Hak;Shin, Dasom;Kang, Hui-Seung
    • Food Science of Animal Resources
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    • v.38 no.5
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    • pp.1055-1063
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    • 2018
  • The aim of study was to investigate the correlation between the level of 17 antibiotic residues and 6 antibiotic resistances of Escherichia coli isolates in chicken meats. A total of 58 chicken meats were collected from retail grocery stores in five provinces in Korea. The total detection rate of antibiotic residues was 45% (26 out of 58). Ten out of 17 antibiotics were detected in chicken meats. None of the antibiotics exceeded the maximum residue level (MRLs) in chicken established by the Ministry of Food and Drug Safety (MFDS). The most detected antibiotics were amoxicillin (15.5%), followed by enrofloxacin (12.1%) and sulfamethoxazole (10.3%). In a total of 58 chicken meats, 51 E. coli strains were isolated. E. coli isolates showed the highest resistance to ampicillin (75%), followed by tetracycline (69%), ciprofloxacin (65%), trimethoprim/sulfamethoxazole (41%), ceftiofur (22%), and amoxicillin/clavulanic acid (12%). The results of study showed basic information on relationship between antibiotic residue and resistance for 6 compounds in 13 chicken samples. Further investigation on the antibiotic resistance patterns of various bacteria species is needed to improve food safety.

Reduction Rate of Azoxystrobin, Fenhexamid and Cyprodinil during Ginseng Processing (홍삼 가공중 azoxystrobin, fenhexamid 및 cyprodinil농약의 감소율)

  • Im, Moo-Hyeog;Kwon, Kwang-Il;Park, Kun-Sang;Lee, Kyung-Jin;Chang, Moon-Ik;Yun, Won-Kap;Choi, Woo-Jong;Yoo, Kwang-Soo;Hong, Moo-Ki
    • Korean Journal of Food Science and Technology
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    • v.39 no.5
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    • pp.575-579
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    • 2007
  • This study was performed to acquire scientific data for establishing the maximum residue limits (MRLs) of pesticides in Korean red ginseng and its extract. Pesticides (azoxystrobin, fenhexamid, cyprodinil) were applied to a cultivated field of ginseng, and the fresh ginseng was harvested and processed to make Korean red ginseng and its extract. The reduction rates of the residue pesticides were calculated by determining the pesticide contents in each stage of ginseng processing. The residue levels in fresh ginseng were 0.12 ppm for azoxystrobin, 0.19 ppm for fenhexamid, and 1.78 ppm for cyprodinil. The residue levels in Korean red ginseng were 0.24, 0.54, and 1.49 ppm, and in the extract 0.81, 1.93, and 3.66 ppm for azoxystrobin, fenhexamid, and cyprodinil, respectively. The steaming and processing of fresh ginseng increased azoxystrobin and fenhexamid residues, but cyprodinil was reduced. The reduction rates (dry basis) of azoxystrobin, fenhexamid, and cyprodinil were 0.66, 0.94, and 0.28 for Korean red ginseng, and 3.25, 4.94, and 1.01 for the extract, respectively.

Liquid Chromatographic Determination of Etofenprox Residues in Foods with Mass-Spectrometric Confirmation

  • Lee, Young-Deuk;Kwon, Chan-Hyeok;Kwon, Ki-Sung
    • Korean Journal of Environmental Agriculture
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    • v.30 no.4
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    • pp.432-439
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    • 2011
  • BACKGROUND: An official analytical method was developed to determine etofenprox residues in agricultural commodities using high-performance liquid chromatography (HPLC). METHODS AND RESULTS: The etofenprox residue was extracted with acetone from representative samples of five raw products which comprised rice grain, apple, mandarin, cabbage, and soybean. The extract was then serially purified by liquid-liquid partition and Florisil column chromatography. For rice and soybean samples, acetonitrile/n-hexane partition was additionally coupled to remove nonpolar lipids. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate etofenprox from co-extractives. Intact etofenprox was sensitively detected by ultraviolet absorption at 225 nm. Recovery experiment at the quantitation limit validated that the proposed method could apparently determine the etofenprox residue at 0.02 mg/kg. Mean recoveries from five crop samples fortified at three levels in triplicate were in the range of 93.6~106.4%. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types. A selected-ion monitoring LC/mass spectrometry with positive atmospheric-pressure chemical ionization was also provided to confirm the suspected residue. CONCLUSION(s): The proposed method is simple, rapid and sensitive enough to be employed in routine inspection or monitoring of agricultural products for the etofenprox residue.

Determination of Ceftiofur Residues by Simple Solid Phase Extraction Coupled with Liquid Chromatography-Tandem Mass Spectrometry in Eel, Flatfish, and Shrimp

  • Kim, Joohye;Shin, Dasom;Kang, Hui-Seung;Lee, Eunhye;Choi, Soo Yeon;Lee, Hee-Seok;Cho, Byung-Hoon;Lee, Kang-Bong;Jeong, Jiyoon
    • Mass Spectrometry Letters
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    • v.10 no.2
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    • pp.43-49
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    • 2019
  • The aim of this study was conducted to develop an analytical method to determine the concentration of ceftiofur residue in eel, flatfish, and shrimp. For derivatization and extraction, the sample was hydrolyzed with dithioerythritol to produce desfuroylceftiofur, which was then derivatized by iodoacetamide to obtain desfuroylceftiofur acetamide. For purification, the process of solid phase extraction (Oasis HLB) was used. The target analytes were confirmed and quantified in $C_{18}$ column using liquid chromatography-tandem mass spectrometry with 0.1% formic acid in water (A) and 0.1% formic acid in acetonitrile (B) as the mobile phase. The linearity of the standard calibration curve was confirmed by a correlation coefficient, $r^2>0.99$. The limit of quantification for ceftiofur was 0.002 mg/kg; the accuracy (expressed as the average recoveries) was 80.6-105%; the precision (expressed as the coefficient of variation) was below 6.3% at 0.015, 0.03, and 0.06 mg/kg. The validated method demonstrated high accuracy and acceptable sensitivity to meet the Codex guideline requirements. The developed method was tested using market samples. As a results, ceftiofur was detected in one sample. Therefore, it can be applied to the analysis of ceftiofur residues in fishery products.