• Fisheries and Aquatic Sciences
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• v.22 no.12
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• pp.29.1-29.7
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• 2019

Veterinary drugs are widely used to protect production-related diseases and promote the growth of farmed fish. The use of large amounts of veterinary drugs may have potential risk and cause adverse effects on both humans and the environment. In this study, we developed risk-based ranking based on a scoring system to be applied in the national residue program. In this approach, the following three factors of veterinary drugs that may occur as residues in fishery products were considered: potency (acceptable daily intake), usage (number of dose and withdrawal period), and residue occurrence. The overall ranking score was calculated using the following equation: potency × usage (sum of the number of sales and withdrawal period) × residue occurrence. The veterinary drugs that were assigned high score by applying this approach were enrofloxacin, amoxicillin, oxolinic acid, erythromycin, and trimethoprim. The risk-based approach for monitoring veterinary drugs can provide a reliable inspection priority in fishery products. The developed ranking system can be applied in web-based systems and residuemonitoring programs and to ensure safe management of fishery products in Korea.

• 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.

• 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.

• 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.

• 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.

• Food Science of Animal Resources
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• v.43 no.5
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• pp.914-937
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• 2023

The objective of this study was to establish a multi-residue quantitative method for the analysis of anthelmintic and antiprotozoal drugs in various livestock products (beef, pork, and chicken) using ultra-high-performance liquid chromatography-tandem mass spectrometry. Each compound performed validation at three different levels i.e., 0.5, 1, and 2× the maximum residue limit according to the CODEX guidelines (CAC/GL 71-2009). This study was conducted according to the modified quick, easy, cheap, effective, rugged, and safe procedure. The matrix-matched calibrations gave correlation coefficients >0.98, and the obtained recoveries were in the range of 60.2%-119.9%, with coefficients of variation ≤32.0%. Furthermore, the detection and quantification limits of the method were in the ranges of 0.03-3.2 and 0.1-9.7 ㎍/kg, respectively. Moreover, a survey of residual anthelmintic and antiprotozoal drugs was also carried out in 30 samples of beef, pork, and chicken collected in Korea. Toltrazuril sulfone was detected in all three samples. Thus, our results indicated that the developed method is suitable for determining the anthelmintic and antiprotozoal drug contents in livestock products.

• Korean Journal of Environmental Agriculture
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• v.30 no.1
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• pp.89-97
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• 2011

BACKGROUND: Cypermethrins, possess eight isomers, used both as pesticide and as veterinary drug, were set different MRLs for livestock by CCPR and CCRVDF of Codex Alimentarius. Korea Food Code designates MRLs for livestock only as pesticide. METHODS AND RESULTS: This study presented necessaries of harmonization of MRL setting for compounds used both as pesticides and as veterinary drugs with regulatory aspects, showing an example of cypermethrin residue in livestock. CONCLUSION(S): For harmonization, following factors must be considered and recommended; designation of marker residue; alpha-cypermethrin, zeta- cypermethrin, and cypermethrin, clarification of the definition of target tissues; meat, fat, muscle, by-product, eggs, milk, and etc., method of analysis; clarification of target analytes of isomers, quantitation and calculation method as a principle of residue analysis.

• Asian-Australasian Journal of Animal Sciences
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• v.12 no.2
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• pp.233-243
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• 1999

Food safety or sanitation are terms broadly applicable to procedures designed to ensure that food quality is high and free of factors which may adversely affect human health. These factors include zoonotic diseases and acute and chronic effects of ingesting natural and human-made xenobiotics. Use of drugs in animal production for the treatment and control of animal diseases, to promote growth rate, and to improve feed conversion efficiency has expanded year by year, thus increasing the possibilities for occurrences in animal products of residues harmful to humans. Governmental agencies have made efforts to control or prevent residue problems. The Korean Food and Drug Administration (KFDA) is charged with the responsibility of establishing tolerances for veterinary drugs, pesticides, and mycotoxins and other non-pharmaceutical substances. The Department of Veterinary Service is responsible for establishing guidelines regarding withdrawal times of drugs, approval of drugs, their uses, and sanitation enforcement of livestock products. The authors describe the toxicological basis for the establishment of tolerance levels for xenobiotics and the pharmacokinetic basis for establishing withdrawal time for veterinary drugs. The regulatory tolerance levels of chemicals in pork and swine feed, Korean regulations on the use of feed additives, rapid residue test methods, the National Residue Program, and the Food Animal Residue Avoidance Databank are discussed. Rapid EIA methods that are under development for the screening of live animals are described These methods predict tissue residues from an examination of blood samples taken from pigs before they are slaughtered.

• Analytical Science and Technology
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• v.28 no.3
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• pp.175-181
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• 2015

Cyantraniliprole, which is an ananthranilic diamide insecticide that was developed by the DuPont Corporation, was registered in the Republic of Korea in 2012. It offers exceptional insecticidal activity on a broad range of Lepidopera, Coleoptera, Diptera, and Isoptera. The maximum residue limits are set to pepper, peach, apple, sweet pepper, welsh onion, and so on (0.2~2.0 mg/kg). Therefore, an analytical method for determining cyantraniliprole residue in agricultural products was developed to ensure food safety. In previous studies, welsh onions were among vegetables included in the allium species, which is a representative plant with sulfur organic compounds. In this study, the analytical method was developed and evaluated for the elimination of sulfur compounds from the test solution of allium species during pesticide residue analysis. In order to inactivate the enzyme allinase and produce sulfur compounds, sample extraction was made in the base state pH 10 by reducing the activity of the enzyme. The recoveries of the developed method ranged from 81.9% to 83.2%, and the relative standard deviations were less than 10%. Therefore, based on the results, the method developed in this study is accurate and appropriate for use in cyantraniliprole determination. It will be used as the official method for managing the safety of cyantraniliprole residues in agricultural products.

• Korean Journal of Environmental Agriculture
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• v.34 no.2
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• pp.111-119
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• 2015

BACKGROUND: Ethychlozate (ECZ) is a plant growth regulator of synthetic auxin for agricultural commodities (ACs). Accurate and sensitive method to determine ECZ in diverse ACs on global official purpose is required to legal residue regulation. As the current official method is confined to the limited type of crops with poor validation, this study was conducted to improve and extend the ECZ method using high-performance liquid chromatography (HPLC) in all the registered crops with method verification. METHODS AND RESULTS: ECZ and its acidic metabolite (ECZA) were both extracted from acidified samples with acetone and briefly purified by dichloromethane partition. ECZ was hydrolyzed to form ECZA and the combined ECZA was finally purified by ion-associated partition including hexane-washing. The instrumental quantitation was performed using HPLC/ FLD under ion-suppression of ECZA with no interference by sample co-extractives. The average recoveries of intra- and inter-day experiment ranged from 82.0 to 105.2% and 81.7 to 102.8%, respectively. The repeatability and reproducibility for intra- and inter-day measurements expressed as a relative standard deviation was less than 8.7% and 7.4%, respectively. CONCLUSION: Established analytical method for ECZ residue in ACs was applicable to the nation-wide pesticide residues monitoring program with the acceptable level of sensitivity, repeatability and reproducibility.