• Korean Journal of Veterinary Research
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• v.62 no.2
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• pp.18.1-18.8
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• 2022

This study investigated dexamethasone (DXM) residues in the milk from intramuscularly dosed dairy cows and established the withdrawal time (WT) of DXM in milk. Eighteen healthy Holstein cows were injected with 20 (DXM-1) or 40 mL (DXM-2) of a drug containing 1 mg/mL of DXM. After administering DXM, milk samples were collected from all cows at 12-hour intervals for five days. The DXM residue concentrations in milk were determined by liquid chromatography-tandem mass spectrometry. The correlation coefficient of the calibration curve was 0.9966, and the limits of detection and quantification (LOQ) were 0.03 and 0.1 ㎍/kg, respectively. The recoveries were 97.0% to 104.0%, and the coefficient of variations was less than 7.22%. After treatment, DXM in DXM-1 was detected above the LOQ in two milk samples at 36 hours and below the LOQ in all milk samples of DXM-2 at 48 hours. Using the WT calculation program WT 1.4, the withdrawal periods of DXM-1 and DXM-2 in milk were established to be two days. In conclusion, the developed analytical method is sensitive and reliable for detecting DXM in milk. The estimated WT of DXM in bovine milk is shorter than the current milk WT recommendation of three days for DXM in lactating dairy cows.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.235-241
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• 2019

An analytical method was developed for the determination of an antibiotic fungicide, kasugamycin, in agricultural products (hulled rice, potato, soybean, mandarin and green pepper) using liquid chromatographytandem mass spectrometry (LC-MS/MS). Samples were extracted with methanol adjusted to pH 13 using 1 N sodium hydroxide, and purified with a HLB (hydrophilic lipophilic balance) cartridge. Linearity of a matrix-matched calibration curve using seven concentration levels, from 0.001 to 0.1 mg/kg, was excellent with a correlation coefficient ($R^2$) of more than 0.9998. The limits of detection (LOD) and quantification (LOQ) of instrument were 0.0005 and $0.001{\mu}g/mL$, respectively, and the LOQ of analytical method calculated as 0.01 mg/kg. The average recoveries at three spiking levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) were in the range of 71.2~95.4% with relative standard deviation of less than 12.1%. The developed method was simple and all optimized results was satisfied with the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. The present study could be served as a reference for the establishment of maximum residue limits (MRL) of kasugamycin and be used as basic data for safety management relative to kasugamycin residues in imported and domestic agricultural products.

• Korean Journal of Environmental Agriculture
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• v.32 no.3
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• pp.214-223
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• 2013

BACKGROUND: This study focused on the development of an analytical method about dichlorprop (DCPP; 2-(2,4-dichlorophenoxy)propionic acid) which is a plant growth regulator, a synthetic auxin for agricultural commodities. DCPP prevents falling of fruits during their growth periods. However, the overdose of DCPP caused the unwanted maturing time and reduce the safe storage period. If we take fruits with exceeding maximum residue limits, it could be harmful. Therefore, this study presented the analytical method of DCPP in agricultural commodities for the nation-wide pesticide residues monitoring program of the Ministry of Food and Drug Safety. METHODS AND RESULTS: We adopted the analytical method for DCPP in agricultural commodities by gas chromatograph in cooperated with Electron Capture Detector(ECD). Sample extraction and purification by ion-associated partition method were applied, then quantitation was done by GC/ECD with DB-17, a moderate polarity column under the temperature-rising condition with nitrogen as a carrier gas and split-less mode. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.9998, analysed from 0.1 to 2.0 mg/L concentration. Limit of quantitation in agricultural commodities represents 0.05 mg/kg, and average recoveries ranged from 78.8 to 102.2%. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 9.5% in 0.05, 0.10, and 0.50 mg/kg. CONCLUSION(S): Our newly improved analytical method for DCPP residues in agricultural commodities was applicable to the nation-wide pesticide residues monitoring program with the acceptable level of sensitivity, repeatability and reproducibility.

• Korean Journal of Food Science and Technology
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• v.42 no.6
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• pp.643-647
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• 2010

This research was carried out to investigate residues of neomycin, streptomycin, dihydrostreptomycin, amitraz, 2,4-dimethylaniline (one of amitraz's metabolites), and coumaphos in honey in order to intensively control their use following the establishment of Korean maximum residue limits (MRLs) for veterinary drugs in honey in 2007. To monitor for residues, 110 honeys and food products with honey were collected and analyzed. The collected honeys included acasia, mixed flower, chestnut, rape flower, jujube, and native types. Neomycin, streptomycin, dihydrostreptomycin, oxytetracycline, and amitraz were not detected among samples. Coumaphos was found in the Korean acasia honey at 0.02 mg/kg, but its concentration was under the MRL (0.1 mg/kg) for coumaphos. According to the results, there were no violations of the Korean MRLs of veterinary drugs in honey.

• Journal of Food Hygiene and Safety
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• v.31 no.3
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• pp.186-193
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• 2016

An analytical method was developed for the determination of oxathiapiprolin in agricultural commodities. Oxathiapiprolin is a new oomycide (fungicide of piperidinyl thiazole isoxazoline class) which controls downy mildew in cucurbits caused by Pseudoperonospora cubensis (oomycete plant pathogen). Agricultural commodities were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, adjusting pH between 9 and 10 by 1 N sodium hydroxide. After purification by silica SPE cartridge to clean up the interference of organic compounds, they were finally quantified by HPLC-UVD (high performance liquid chromatograph ultraviolet detector) using a wavelength at 260 nm and confirmed by LC-MS (liquid chromatograph mass spectrometer) in electro-spray ionization positive ion mode. The standard calibration curve was linear with coefficients of determination ($r^2$) 1.00 over the calibration ranges (0.025-2.5 mg/L). Recoveries were ranged between 86.7 to 112.7%, with relative standard deviations less than 10% at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates. The overall results were determined and estimated according to the CODEX guidelines (CAC/GL40). The proposed method for determination of oxathiapiprolin residues in agricultural commodities can be used as an official method.

• Korean Journal of Veterinary Research
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• v.36 no.3
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• pp.571-575
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• 1996

Sulfamethazine sodium was orally administrated to Sprague Dawley female rats(body weight: 200~250g) with the sonde caude at the dose of 20mg of sulfamethazine sodium per 100g of body weight for 3 days to investigate the depletion rate of the drug from liver, kidney and muscle of rat. The results obtained were summerized as follows; 1. The mean concentrations of sulfamethazine in liver according to the time lapsed after oral administration of the sulfamethazine sodium were decreased from 1.27ppm at day 1 to 0.28ppm at day 4. 2. Sulfamethazine concentrations in kidney according to the time lapsed after oral administration of the sulfamethazine sodium were decreased from 0.77ppm at day 1 to 0. 12ppm at day 4. 3. The mean concentration of sulfamethazine in skeletal muscle according to the time lapsed after oral administration of the sulfamethazine sodium was at or below 0.09ppm within 4 days after withdrawl of medicated solution.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.210-217
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• 2015

Ipfencarbazone is a herbicide of the tetrazolinone class, and is believed to be an inhibitor of very long chain fatty acids (VLCFAs), which control cell division in weeds. The objective of this study was to develop and validate an official analytical method for ipfencarbazone determination in agricultural products. The ipfencarbazone residues in agricultural products were extracted with acetone, partitioned with n-hexane, and then purified through silica SPE cartridge. Finally, the analyte was quantified by gas chromatograph-electron capture detector (GC-ECD) and confirmed with gas chromatograph/mass spectrometer(GC/MS). The linear range of ipfencarbazone was 0.01 to 1.0 mg/L with the coefficient of determination ($r^2$) of 0.9999. The limit of detection (LOD) and quantification (LOQ) was 0.003 and 0.01 mg/kg, respectively. In addition, average recoveries of ipfencarbazone ranged from 80.6% to 112.3% at the different concentration levels LOQ, 10LOQ and 50LOQ, while the relative standard deviation was 2.2-8.6%. All values were consistent with the criteria ranges requested in the CODEX guidelines. Furthermore, and inter-laboratory study was conducted to validate the method. This proposed method for determination of ipfencarbazone residues in agricultural products can be used as an official analytical method.

• Journal of Food Hygiene and Safety
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• v.29 no.3
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• pp.234-240
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• 2014

Fluxapyroxad is classified as carboxamide fungicide that inhibits succinate dehydrogenase in complex II of mitochondrial respiratory chain, which results in inhibition of mycelial growth within the fungus target species. This study was carried out to assure the safety of fluxapyroxad residues in agricultural products by developing an official analytical method. A new, reliable analytical method was developed and validated using High Performance liquid Chromatograph-UV/visible detector (HPLC-UVD) for the determination of fluxapyroxad residues. The fluxapyroxad residues in samples were extracted with acetonitrile, partitioned with dichloromethane, and then purified with silica solid phase extraction (SPE) cartridge. Correlation coefficient($R^2$) of fluxapyroxad standard solution was 0.9999. The method was validated using apple, pear, peanut, pepper, hulled rice, potato, and soybean spiked with fluxapyroxad at 0.05 and 0.5 mg/kg. Average recoveries were 80.6~114.0% with relative standard deviation less than 10%, and limit of detection (LOD) and limit of quantification (LOQ) were 0.01 and 0.05 mg/kg, respectively. All validation parameters were followed with Codex guideline (CAC/GL 40). LC-MS (Liquid Chromatograph-Mass Spectrometer) was also applied to confirm the analytical method. Base on these results, this method was found to be appropriate fluxapyroxad residue determination and can be used as the official method of analysis.

• Journal of Food Hygiene and Safety
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• v.25 no.3
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• pp.226-231
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• 2010

We aimed at the monitoring medroxyprogesterone acetate (MPA) residue amount in meats and confirmed the safety of its residue in meats. Optimized condition for analytical and instrumental methods was obtained by method validation. The limit of detection (LOD) and limit of quantification (LOQ) were validated at 1.5 and 5.0 ug/kg, respectively. The calibration curve showed good linearity ($r^2$ = 0.9968) within the concentration range of 5.0~50.0 ug/kg. We selected progesterone-d9 for internal standard, The recoveries in fortified meat ranged from 67.5 to 109.56% at the 3 spiking levels. As the regulation of MPA analysis method used by LC-MS/MS on other products have established. We selected 3 species of farm stock products (cattle, pig, chicken) and purchased at the markets of seven major cities. The total 196 of meat including 46 of domestic beef, 43 of import beef, 60 of domestic pork, 12 of import pork and 35 of domestic chicken. No residue of synthetic growth hormones were detected in cattle, pig and chicken samples tested.

• Journal of Food Hygiene and Safety
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• v.28 no.3
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• pp.213-216
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• 2013

Antibiotic Detection Kit (Combination I), a lateral flow immunoassay (LFIA) developed for the detection of antibiotic residues in milk, was utilized for the analysis of antibiotic residues in the muscle tissue of olive flounder. After 60-min treatment by dipping in water dosed with ampicillin (200-g/ton water), the residue depletion of ampicillin was investigated in 25 cultured olive flounder (Paralichthys olivaceus). Muscles of fish were sampled on the 1st, 2nd, 3rd, 4th and 5th day after drug treatment. The concentration of ampicillin in the muscle was determined by LFIA. The absorbance ratio of the sample to the control blank (Bs/Bo) was employed as an index to determine the muscle residues in olive flounder. To investigate the recovery rate, standard solutions were added to muscle samples to give final concentrations in the muscle of 4 and 8 ng/ml. The recovery rates of all spiked samples were > 96% of the spiked value. Ampicillin was detected in the muscle of fish treated with the drug until the 2nd day of the withdrawal period. The present study showed that the LFIA can be easily adopted to predict ampicillin residues in tissue of farmed fishes.