• Korean Journal of Environmental Agriculture
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• v.36 no.3
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• pp.184-192
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• 2017

BACKGROUND: This study was performed to evaluate the residue dissipation of boscalid and spinetoram on crown daisy and sweet pepper affected by the morphology of the crop. The half-lives and dissipation rate constants for boscalid and spinetoram on crown daisy and sweet pepper were calculated. And then lower limit of 95% confidence interval for dissipation rate constant could be used to propose the pre-harvest residue limit. METHODS AND RESULTS: The pesticide products diluted according to the pesticide label were applied one time on crown daisy and sweet pepper at 2 field sites, respectively. Initial concentration of boscalid and spinetoram on crown daisy after application were in the range of 72.80~117.15 mg/kg and 2.82~4.67 mg/kg, respectively. And Initial concentration of boscalid and spinetoram on sweet pepper were in the range of 1.58~1.62 mg/kg and 0.10~0.21 mg/kg, respectively. Boscalid and spinetoram for crown daisy dissipted below the maximum residue limit(MRL) at 10 and 2 days after application, respectively. All residues concentration of boscalid and spinetoram for sweet pepper below the MRL at 0 day after application. The half-lives based on dissipation rate constant for boscalid and spinetoram on crown daisy were 4.2~4.9 days and 3.0~2.4 days respectively. And the half-lives for boscalid and spinetoram on sweet pepper were 6.7~7.0 days and 2.8~4.0 days respectively. CONCLUSION: The difference in initial concentration of boscalid and spinetoram among crop commodities were due to different crop morphology with larger surface areas. This study was suggested that pre-harvest residue limit would be calculated from lower limit of 95% confidence interval for dissipation rate constant and would be useful to protect consumers by controlling the pesticide residues in crop.

• Korean Journal of Veterinary Service
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• v.44 no.3
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• pp.125-131
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• 2021

Benzimidazole is an widely used anthelmintics in livestock clinics. The aim of present study was to investigate benzimidazole residues in the meat in Sejong City. A total of 338 samples of meat(beef 287, pork 37, chicken 14) were selected from the laboratory meat(Korean beef genetic test, hygiene test) supplied to school in Sejong City. Representative benzimidazole class drug such as thiabendazole, 2-amino albendazole sulfone, fenbendazole, oxfendazole, and oxfendazole sulfone were monitored in samples by using lc-ms/ms and the analysis was preformed based on the Korea Food Code guideline. Limit of quantitation (LOQ) was ranged from 0.56 to 3.02 ppb for target drugs and the accuracy was within the acceptance criteria. Among the sample analyzed only one case, the pork meat was found to have drug levels that exceed LOQ. However, the overall residue concentration was 2.17 ppb, which was lower than the maximum residue levels (100 ppb).

• Korean Journal of Environmental Agriculture
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• v.32 no.1
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• pp.70-77
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• 2013

BACKGROUND: Nitroxoline is an antibiotic agent. It is used for the treatment of the second bacterial infection by the colibacillosis, salmonellosis and viral disease of the poultry. When the nitroxoline is indiscreetly used, the problem about the abuse of the antibiotics can occur. Therefore, this study presented the residue analytical method of nitroxoline in food for the safety management of animal farming products. METHODS AND RESULTS: A simple, sensitive and specific method for nitroxoline in chicken muscle by high performance liquid chromatograph with PDA was developed. Sample extraction with acetonitrile, purification with SPE cartridge (MCX) were applied, then quantitation by HPLC with C18 column under the gradient condition with 0.1 % tetrabutylammonium hydroxide-phosphoric acid and methanol was performed. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.999, analysed from 0.02 to 0.5 mg/L concentration. Limit of quantitation in chicken muscle showed 0.02 mg/kg, and average recoveries ranged from 72.9 to 88.1 % in chicken muscle. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 12 % in 0.02 and 0.04 mg/kg. CONCLUSION(S): Newly developed method for nitroxoline in chicken muscle was applicable to food inspection with the acceptable level of sensitivity, repeatability and reproducibility.

• 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.

• Journal of Food Hygiene and Safety
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• v.30 no.3
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• pp.272-280
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• 2015

A simultaneous official method was developed for the determination of phorate and its metabolites (phorate sulfoxide, phorate sulfone, phorate oxon, phorate oxon sulfoxide, phorate oxon sulfone) in livestock samples. The analytes were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Phorate and its metabolites were extracted from beef and milk samples with acidified acetonitrile (containing 1% acetic acid) and partitioned with anhydrous magnesium sulfate. Then, the extract was purified through primary secondary amine (PSA) and C18 dispersive sorbent. Matrix matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/L) for all the analytes into blank extract with $r^2$ > 0.996. For validation purposes, recovery studies were carried out at three different concentration levels (beef 0.004, 0.04 and 0.2 mg/kg; milk 0.008, 0.04 and 0.2 mg/kg, n = 5). The recoveries were within 79.2-113.9% with relative standard deviations (RSDs) less than 19.2% for all analytes. All values were consistent with the criteria ranges requested in the Codex guidelines. The limit of quantification was quite lower than the maximum residue limit (MRL) set by the Ministry of Food and Drug Safety (0.05 mg/kg). The proposed analytical method was accurate, effective and sensitive for phorate and its metabolites determination and it will be used to as an official analytical method in Korea.

• Korean Journal of Veterinary Research
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• v.46 no.3
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• pp.291-294
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• 2006

$Parallux^{TM}$, a solid-phase fluorescence immunoassay(SPFIA) developed for antibiotics residue detection in milk, was applied for analysis of fish muscle. The recommended therapeutic dose of ampicillin(100 mg/kg body weight, withdrawal period 7 days) was orally administered to a group of 25 olive flounders(Paralichthys olivaceus) for consecutive five days. Muscle was sampled after drug treatment 1st, 2nd, 3rd, 4th and 5th day. The concentration of ampicillin in muscle, determined by SPFIA, was compared with that of internal standard(10 ppb as ampicillin). The absorbance ratio of sample to internal standard(Bs/Bo) was employed as an index to determine the muscle residue in olive flounder. To investigate the recovery rate, the standard solutions were added to muscle samples to give final concentrations in muscle of 10 and 50 ng/ml. The recovery rates of all spiked samples were > 89% of the spiked value. Ampicillin was detected in muscle of fishes treated until the 3rd day of withdrawal period. The present study showed that the SPFIA can be easily adopted in predicting tissue residues for ampicillin in farmed fishes.

• Food Science of Animal Resources
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• v.39 no.5
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• pp.687-703
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• 2019

A survey we conducted suggests that the ingestion of veterinary drug residues in edible animal parts constitutes a potential health hazard for its consumers, including, specifically, the possibility of developing multidrug resistance, carcinogenicity, and disruption of intestinal normal microflora. The survey results indicated that antibiotics, parasitic drugs, anticoccidial, or nonsteroidal anti-inflammatory drugs (NSAIDs) are broadly used, and this use in livestock is associated with the appearance of residues in various animal products such as milk, meat, and eggs. We observed that different cooking procedures, heating temperatures, storage times, fermentation, and pH have the potential to decrease drug residues in animal products. Several studies have reported the use of thermal treatments and sterilization to decrease the quantity of antibiotics such as tetracycline, oxytetracycline, macrolides, and sulfonamides, in animal products. Fermentation treatments also decreased levels of penicillin and pesticides such as dimethoate, malathion, Dichlorodiphenyldichloroethylene, and lindane. pH, known to influence decreases in cloxacillin and oxacillin levels, reportedly enhanced the dissolution of antimicrobial drug residues. Pressure cooking also reduced aldrin, dieldrin, and endosulfan in animal products. Therefore, this review provides updated information on the control of drug residues in animal products, which is of significance to veterinarians, livestock producers, and consumer health.

• Asian-Australasian Journal of Animal Sciences
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• v.14 no.3
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• pp.402-413
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• 2001

Food safety is a term broadly applied to food quality that may adversely affect human health. These include zoonotic diseases and acute and chronic effects of ingesting natural and human-made xenobiotics. There are two major areas of concern over the presence of residues of antibiotics in animal-derived foodstuffs with regard to human health. The first is allergic reactions. Some antibiotics, such as penicillins can evoke allergic reactions even though small amounts of them are ingested or exposed by parenteral routes. The second is development of antibiotic resistance in gut bacteria of human. Recently multi-resistant pneumococcal, glycopeptide-resistant enterococci and gram negative bacteria with extended-spectrum $\beta$-lactamases have spread all over the world, and are now a serious therapeutic problem in human. Although it is evident that drugs are required in the efficient production of meat, milk and eggs, their indiscriminate use should never be substituted for hygienic management of farm. Drug should be used only when they are required. In addition to veterinary drugs, environmental contaminants that were contaminated in feed, water and air can make residues in animal products. Mycotoxins, heavy metals, pesticides, herbicides and other chemicals derived from industries can be harmful both to animal and human health. Most of organic contaminants, such as dioxin, PCBs and DDT, and metals are persistent in environment and biological organisms and can be accumulated in fat and hard tissues. Some of them are suspected to have endocrine disrupting, carcinogenic, teratogenic, immunodepressive and nervous effects. The governmental agencies concerned make efforts to prevent residue problems; approval of drugs including withdrawal times of each preparation of drugs, establishment of tolerances, guidelines regarding drug use and sanitation enforcement of livestock products. National residue program is conducted to audit the status of the chemical residues in foods. Recently HACCP has been introduced to promote food safety from farm to table by reducing hazardous biological, chemical and physical factors. Animal Production Food Safety Program, Quality Assurance Programs, Food Animal Residue Avoidance Databank are para- or non-governmental activities ensuring food safety. This topic will cover classification and usage or sources of chemical residues, their adverse effects, and chemical residue status of some countries. Issues are expanded to residue detection methodologies, toxicological and pharmacokinetic backgrounds of MRL and withdrawal time establishments, and the importance of non-governmental activities with regard to reducing chemical residues in food.

• Korean Journal of Environmental Agriculture
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• v.39 no.2
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• pp.130-137
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• 2020

BACKGROUND: Mefentrifluconazole and triticonazole are the triazole fungicides. The maximum residue levels for agricultural products need to be set up. Therefore, development of the official analytical method for determination of mefentrifluconazole and triticonazole residues from agricultural crops was necessary due to safety management, and then a simultaneous analytical method was developed for the determination of mefentrifluconazole and triticonazole in agricultural crops. METHODS AND RESULTS: Samples were extracted using acetonitrile and purified using dispersive solid phase extraction, and then detected with liquid chromatograph-tandem mass spectrometry (LC-MS/MS). Matrix-matched calibration curves (0.0025-0.25 ㎍/mL) were linear into a sample extract with r²>0.99. For validation, the recovery test was carried out at three fortification levels (LOQ, 10 LOQ and 50 LOQ) from agricultural samples. The results for mefentrifluconazole and triticonazole ranged between 92.3 to 115.3% and 91.4 to 108.5%, respectively and RSD (relative standard deviation) values were also below 6.0%. Furthermore, inter-laboratory was conducted to validate the method. CONCLUSION: All values were corresponded with the criteria ranges requested by both the CODEX (CAC/GL 40-1993, 2003) and MFDS guidelines (2016). Therefore, the proposed method can be used as an official analytical method for determination of mefentrifluconazole and triticonazole (triazole fungicides) in the Republic of Korea.

• 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.