• Title/Summary/Keyword: veterinary drug residue

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Development and Validation of a Simultaneous Analytical Method for 5 Residual Pesticides in Agricultural Products using GC-MS/MS (GC-MS/MS를 이용한 농산물 중 잔류농약 5종 동시시험법 개발 및 검증)

  • Park, Eun-Ji;Kim, Nam Young;Shim, Jae-Han;Lee, Jung Mi;Jung, Yong Hyun;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.36 no.3
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    • pp.228-238
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    • 2021
  • The aim of this research was to develop a rapid and easy multi-residue method for determining dimethipin, omethoate, dimethipin, chlorfenvinphos and azinphos-methyl in agricultural products (hulled rice, potato, soybean, mandarin and green pepper). Samples were prepared using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and analyzed using gas chromatography-tandem mass spectrometry (GC-MS/MS). Residual pesticides were extracted with 1% acetic acid in acetonitrile followed by addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium acetate. The extracts were cleaned up using MgSO4, primary secondary amine (PSA) and octadecyl (C18). The linearity of the calibration curves, which waas excellent by matrix-matched standards, ranged from 0.005 mg/kg to 0.3 mg/kg and yielded the coefficients of determination (R2) ≥ 0.9934 for all analytes. Average recoveries spiked at three levels (0.01, 0.1, 0.5 mg/kg) and were in the range of 74.2-119.3%, while standard deviation values were less than 14.6%, which is below the Codex guideline (CODEX CAC/GL 40).

Application of a solid-phase fluorescence immunoassay to determine streptomycin residues in muscle tissue of olive flounder (Paralichthys olivaceus), rockfish (Sebastes schlegeli), and red sea bream (Pagrus major)

  • Chung, Hee Sik;Kim, Suk;Chun, Myung Sun;Jung, Won Chul;Kim, Dong Hyeok;Shon, Ho Yeong;Lim, Jeong Ju;Lee, Hu-Jang
    • Korean Journal of Veterinary Research
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    • v.47 no.2
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    • pp.241-245
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    • 2007
  • Parallux (IDEXX Laboratories, USA), a solid-phase fluorescence immunoassay (SPFIA) developed for antibiotics residue detection in milk, was applied for analysis of antibiotics in muscle tissue of olive flounder (Paralichthys olivaceus), rockfish (Sebastes schlegeli), and red sea bream (Pagrus major). Fishes were dipped in streptomycin 20 g/ton water, the recommended therapeutic dose, for 3 consecutive days. Muscle was sampled after 1st, 2nd, 3rd, 4th and 5th day drug treatment. The concentration of streptomycin in muscle, determined by SPFIA, was compared with that of internal standard (200 ppb as streptomycin). The absorbance ratio of sample to internal standard (S/C) was employed as an index to determine the muscle residues in fishes. The standard solutions were added to muscle samples to give final concentrations in muscle of 0.2 and 0.5 mg/ml to investigate the recovery rate. The recovery rates of all spiked samples were > 84% of the spiked value. Streptomycin was detected in muscles of fishes treated after the 1st day of withdrawal period. The present study showed that the SPFIA can be easily adopted in predicting muscle tissue residues for streptomycin in farmed fishes.

QuEChERS-based determination of tissue residues and acute toxicity of pyraclofos in rat (QuEChERS 법을 이용한 Rat 조직내 Pyraclofos 잔류 분석 및 급성독성 평가)

  • Pyo, Min-Jung;Hah, Do-Yun;Choi, You-Jeong;Jeong, Kwi-Ok;Han, Chang-Hee;Park, Young-Ho;Kim, Min-Hee;Kim, Won-Gyu;Jung, Jing-Gune;Kim, Munki;Kim, Euikyung
    • Korean Journal of Veterinary Service
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    • v.38 no.3
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    • pp.173-180
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    • 2015
  • Environmental pesticides used for insect control can be transferred from plants to animals even to livestock animals through food chain. Human beings also can be exposed to pesticides by consuming polluted dairy products, including meats, eggs and other milk products. Therefore, the Ministry of Food and Drug Safety (MFDS) established Standard for Pesticide Residue Limits in dairy products. The QuEChERS (quick, easy, cheap, effective, rugged and safe) methods for detecting residual pesticides are relatively well established for fruits and vegetables, however, the methods for meat have not been appropriately studied yet. In the present work, pyraclofos was used as an organophosphate pesticide to examine its tissue residue in experimental animals by QuEChERS methods. For this, pyraclofos (150 mg/kg body weight) was orally administered to male rats once a day for 2 days. After 6, 12, and 24 hr of the treatment, the tissue residues in liver and femoral muscle of the rats were determined using QuEChERS methods followed by HPLC analyses. In preliminary studies, the recovery rates of spiking samples of pyraclofos demonstrated approximately 109~110% from the tissues. In previous study, pyraclofos tissue residues were observed with significantly high levels in livers and muscles at 6 hr of oral treatment. Then, they were almost completely disappeared after 24 hr of the administration, indicating the orally exposed pyraclofos is rapidly absorbed and distributed to body organs, then quickly excreted from the body with a negligible level of tissue residue. The alterations in blood chemistry as well as the histopathology of heart, lung, liver, spleen and kidney have also been investigated in the experimental animals for assessing acute toxic effects of pyraclofos. The obtained blood chemistry indexes (ALT and AST) showed maximum peak values at 12 hr after the oral administration and decreased to the normal levels at 24 hr of the treatment. Histopathologic observation exhibited acute hepatic damages at 24 hr of the treatment. In conclusion, we suggest that QuEChERS method can be adequately optimized for the analysis of pyraclofos residues in animal tissues.

Determination of Nitarsone in Pork, Egg, Milk, Halibut, Shrimp, and Eel Using QuEChERS and LC-MRM

  • Kim, Jin Hee;Jang, Yong Jin;Kim, Dong Yoon;Lee, Hyo Chun;Choi, Yong Seok
    • Mass Spectrometry Letters
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    • v.12 no.1
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    • pp.11-15
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    • 2021
  • Nitarsone is an organoarsenic antiprotozoal drug widely used to treat blackhead disease in turkeys and chickens. However, since its biological conversion into inorganic arsenic, a carcinogen was known, its residue in foods should be regulated. Thus, here, a novel method to determine residual nitarsone in various food commodities (pork, milk, egg, halibut, eel, and shrimp) using QuEChERS and LC-MRM was developed. The developed method was successfully validated through specificity, linearity (coefficient of determination, at least 0.991), recovery (R, 63.6 - 85.6%), precision (the relative standard deviation of R, 0.5 - 10.6%), and sensitivity (the lower limit of quantitation, 5 ppb) by following the Ministry of food and drug safety (MFDS) guidelines. The present method is the first mean to quantitate nitarsone using LC-MRM, and it was designed to be conveniently merged into a new method to quantitate multiple veterinary drugs for the positive list system (PLS). Therefore, the present method could contribute to fortify the food safety system in South Korea.

A study on trend of residual changes in blood and eggs of laying hens after oral administration of quinolones (산란계에서 퀴놀론계 약물투여 후 혈장 및 계란내의 잔류함량 변화추이 조사)

  • Sim Ea-Ran;Kim Mi-Hee;Yoo Eun-Ah;Lee Yun-Jung;Chun Soon-Yong;Moon Soo-Pyeong;Hahm Yoo-Sik
    • Korean Journal of Veterinary Service
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    • v.28 no.3
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    • pp.245-251
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    • 2005
  • The purposes of this study were to evaluate the distribution of quinolone and to investigate the effects of quinolones (enrofloxacin, ciprofloxacin) in blood(plasma) and eggs of laying hens. Animals were fed quinolones which supplemented with 20, 50, 80 mg/kg of body weight. Blood and egg samples were collected after oral administration and analyzed for quinolones (enrofloxacin, ciprofloxacin) by HPLC. In laying hens, the residue period of enrofloxacin were longer than that of ciprofloxacin and the levels of residues were elavated by drug dosage.

Abiraterone Acetate Attenuates SARS-CoV-2 Replication by Interfering with the Structural Nucleocapsid Protein

  • Kim, Jinsoo;Hwang, Seok Young;Kim, Dongbum;Kim, Minyoung;Baek, Kyeongbin;Kang, Mijeong;An, Seungchan;Gong, Junpyo;Park, Sangkyu;Kandeel, Mahmoud;Lee, Younghee;Noh, Minsoo;Kwon, Hyung-Joo
    • Biomolecules & Therapeutics
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    • v.30 no.5
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    • pp.427-434
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    • 2022
  • The drug repurposing strategy has been applied to the development of emergency COVID-19 therapeutic medicines. Current drug repurposing approaches have been directed against RNA polymerases and viral proteases. Recently, we found that the inhibition of the interaction between the SARS-CoV-2 structural nucleocapsid (N) and spike (S) proteins decreased viral replication. In this study, drug repurposing candidates were screened by in silico molecular docking simulation with the SARS-CoV-2 structural N protein. In the ChEMBL database, 1994 FDA-approved drugs were selected for the in silico virtual screening against the N terminal domain (NTD) of the SARS-CoV-2 N protein. The tyrosine 109 residue in the NTD of the N protein was used as the center of the ligand binding grid for the docking simulation. In plaque forming assays performed with SARS-CoV-2 infected Vero E6 cells, atovaquone, abiraterone acetate, and digoxin exhibited a tendency to reduce the size of the viral plagues without affecting the plaque numbers. Abiraterone acetate significantly decreased the accumulation of viral particles in the cell culture supernatants in a concentration-dependent manner. In addition, abiraterone acetate significantly decreased the production of N protein and S protein in the SARS-CoV-2-infected Vero E6 cells. In conclusion, abiraterone acetate has therapeutic potential to inhibit the viral replication of SARS-CoV-2.

Monitoring and Exposure Assessment of Pesticide Residues in Domestic Agricultural Products (국내 유통 다소비 농산물의 잔류농약 모니터링 및 노출평가)

  • Kang, Namsuk;Kim, Seongcheol;Kang, Yoonjung;Kim, Dohyeong;Jang, Jinwook;Won, Sera;Hyun, Jaehee;Kim, Dongeon;Jeong, Il-Yong;Rhee, Gyuseek;Shin, Yeongmin;Joung, Dong Yun;Kim, Sang Yub;Park, Juyoung;Kwon, Kisung;Ji, Youngae
    • The Korean Journal of Pesticide Science
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    • v.19 no.1
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    • pp.32-40
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    • 2015
  • This study was implemented to evaluate food safety on residual pesticides in agricultural products of Korea and to use as a data base for the establishment of food policy. A total of 196 pesticide upon these products were analyzed using multi class pesticide multiresidue methods of Korean Food Code, and 232 samples of 15 agricultural products collected from 9 regions were supplied for this study. In the results, 64 kinds of pesticides were detected in 53 samples, chlorpyrifos and procymidone of them were shown a high frequency of detection in the analyzed pesticides. Among them, two samples (chlorpyrifos in perilla leaves and picoxystrobin in peach) were detected over Maximum Residue Limits (MRLs). The levels of the detected pesticide residues were within safe levels. Also, the intake assessment for pesticide residues including chlorpyrifos at multi pesticide residue monitoring were carried out. The result showed that the ratio of EDI (estimated daily intake) to ADI (acceptable daily intake) was 0.001~0.902% which means that the detected pesticide residues were in a safe range so that residual pesticides in the agricultural products in Korea are properly controlled.

Analysis of antibiotic residues in milk from healthy dairy cows treated with bovine mastitis ointment using ultra-performance liquid chromatography coupled with electrospray tandem mass spectrometry

  • Park, Eun-Kee;Ryu, Yong-Jae;Cha, Chun-Nam;Yoo, Chang-Yeul;Kim, Suk;Lee, Hu-Jang
    • Korean Journal of Veterinary Research
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    • v.56 no.4
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    • pp.233-239
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    • 2016
  • This study was conducted to analyze penicillin G (PEG), streptomycin (STR) and neomycin (NEO) residues in milk of healthy lactating cows. Milk samples were collected from all four quarters of 12 dairy cows 2−7 days after intramammary infusions of an ointment containing PEG, STR and NEO once (n = 4; group I) or twice (n = 4, group II) daily. Ultra-performance liquid chromatography coupled with electrospray tandem mass spectrometry was used to determine the antibiotic residues in the samples. The correlation coefficient ($r^2$) of the calibration curves for all antibiotics was > 0.999 and the limits of detection and quantification were $0.002-0.005{\mu}g/mL$ and $0.007-0.02{\mu}g/mL$, respectively. Recovery rates were ranged from 75.5 to 92.3%. In group I, PEG, STR and NEO residues were detected in milk at 2, 3 and 2 days post-treatment, respectively, which were below the maximum residue limit (MRL). In group II, PEG, STR and NEO residues were detected in milk at 2, 3 and 3 days post-treatment, respectively, which were bellow the MRL. These results suggest that a 3-day for milk withdrawal period after the ointment treatment might be sufficient for reduction of the antibiotic residues below the MRL.

Levels of sulfonamides for animals in food (식품 중 설폰아마이드계 동물용의약품의 잔류실태)

  • Jeong, Jiyoon;Hong, Mooki;Choi, Dongmi
    • Analytical Science and Technology
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    • v.20 no.1
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    • pp.84-90
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    • 2007
  • To determine levels of 11 sulfonamides for animals in food, simultaneously, a selective method of high performance liquid chromatography with UV detector has been applied. The targets were sulfachlorpyridazine (SCP), sulfadiazine (SDZ), sulfadimethoxine (SDM), sulfisoxazole (SSX), sulfamerazine (SMZ), sulfamethazine (SMT), sulfamethoxazole (SMX), sulfamethoxypyridazine (SMP), sulfamonomethoxine (SMM), sulfaquinoxaline (SQX) and sulfathiazole (STZ). Food samples were beef, pork, chicken, milk and whole egg that were collected at the main 6 cities in Korea as Seoul, Busan, Daejon, Incheon, Mokpo and Gangneung. After homogenizing food samples with sodium phosphate solution and acetonitrile, it was extracted with n-hexane. The mobile phase gradient was a mixture of 5 mM potassium phosphate (pH 3.25) and methanol with a gradient ratio from 100:0 to 30:70. The UV wavelength was 270 nm. The overall recoveries were ranged from 75% to 95% and the limit of detection was minimum 0.004 mg/kg for SMT, and 0.007 mg/kg for STZ at signal/noise > 3, respectively. As results, sulfonamide drugs were not detected in most of the selected food samples, however, sulfamonomethoxine was detected in meat. The determined level of sulfamonomethoxine were 0.03 and 0.06 mg/kg for beef that were below the MRLs.

Simultaneous Determination and Monitoring of Three Macrolide Antibiotics in Foods by HPLC (Macrolide계 항생물질 동시분석법 확립 및 모니터링)

  • Park, Sang-Ouk;Lee, Sang-Ho;Ahn, Jong-Hoon;Jung, Young-Ji;Kim, Seong-Cheol;Kim, Ji-Yeon;Keum, Eun-Hee;Sung, Ju-Hyun;Kim, Sang-Yub;Jang, Young-Mi;Kang, Chan-Soon
    • Korean Journal of Food Science and Technology
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    • v.42 no.3
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    • pp.287-291
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    • 2010
  • In this study, a simple and rapid pre-treatment method based on liquid extraction was applied for the simultaneous determination of three macrolides (spiramycin, tylosin, and tilmicosin) residues. In these studies, the stock farm products was used as a matrix sample. When the liquid extraction method was compared with the solid phase extraction (SPE) method, the former showed higher recovery percentages and simpler steps than the latter. The macrolids were separated using a reverse-phase C18 ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$) column and a gradient elution with mobile phases consisting of phosphate buffer (pH 2.5) and acetonitrile. Tylosin and tilmicosin were detected at 288 nm and spiramycin was detected at 232 nm. The average recovery percentage ranged between 83.0-90.2% for samples spiked with the three macrolids at 50 and 100 ng/g The validation results showed that the limit of detection (7 (spiramycin), 12 (tilmiconsin), 12 (tylosin) ng/g)) was under the regulatory tolerances and the linearity from calibration curves was satisfactory for determining the multi-residue of three macrolids in farm products. Monitoring samples were collected at the main cities in Korea as Seoul, Busan, Deajeon, Incheon, Deagu, and Gwangju. Microlide antibiotics were not detected in most samples.