• Journal of Applied Biological Chemistry
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• v.64 no.2
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• pp.177-184
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• 2021

While veterinary antibiotics are used only in a part of the dose administered, the rest are excreted as urine or feces. Residual antibiotics enter the adjacent agricultural environments by spraying manure-based composts on farmlands and lead to secondary pollution. Therefore, it is necessary to develop the technique for post management such as regulatory levels of antibiotics in the agricultural environments. This study was conducted to compare by different matrices the amount of residual antibiotics such as tetracyclines and sulfonamides, which are known to be frequently used in Korea and to practice risk assessment by different antibiotics in soils before and after application of composts. Pre-treatment with modified typical method using buffer and solid phase extraction showed the recovery of composts and soils was more than 70% at ppb level and the limits of detection were 0.13-0.46 and 0.05-0.25 ㎍/kg, respectively. Analysis of manure-based composts revealed concentrations from 5.38 to 196.0 ㎍/kg for tetracyclines, from below the detection of limit (BDL) to 259.0 ㎍/kg for sulfonamides. In case of agricultural soils, residual concentrations of selected veterinary antibiotics were ranged 0.30-53.3 ㎍/kg, BDL-4.16 ㎍/kg respectively and the concentration level of tetracyclines, which had higher soil distribution coefficient (Kd) values, was higher than that of sulfonamides. There was a difference in human risk assessment by different antibiotics in soil before and after application of composts. But, it was indicated that detection values of all of 5 antibiotics were very safe on the basis that Hazard Quotient was safe below 1.

• Korean Journal of Food Science and Technology
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• v.26 no.3
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• pp.221-225
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• 1994

This survey was carried out to determine five sulfonamide(sulfamerazine, sulfamethazine, sulfadimethoxine, sulfamonomethoxine, sulfaquinoxaline) residues in beef, pork, chicken and swine kidney. For this survey, 30 samples of beef, 15 samples of chicken, 10 samples of pork and 10 samples of swine kidney were collected in Chonnam from June, 1992 to June, 1993, and were analyzed by HPLC. The recoveries of sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfadimethoxine, and sulfaquinoxaline in spiked samples between $0.25{\sim}1.00$ ppm were 71.7%, 80.3%, 71.6%, 70.9%, 68.4%, respectively. None of 65 samples which were examined exceeded 0.1 ppm. Of 15 chicken muscle samples, 2 samples exceeded 0.05 ppm in sulfamerazine (0.077 ppm) and sulfamethazine (0.075 ppm), respectively. Of 10 swine kidney samples, 1 sample exceeded 0.05 ppm in sulfadimethoxine (0.052 ppm). And sulfanilamide concentration of swine kidney were higher than pork.

• Food Science and Biotechnology
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• v.18 no.6
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• pp.1430-1434
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• 2009

The present study used the liquid extraction pretreatment method and developed a liquid chromatographyultraviolet detector (LC-UV) for the simultaneous determination of 14 sulfonamides (SAs) residues in porcine and chicken muscle. Linearity within a range of $50-150\;{\mu}g/kg$ was obtained with the correlation coefficient ($r^2$) of 0.9673-0.9997. The mean recovery of SAs was 55.9-109.7% (relative standard deviations; RSDs 1.7-17.3%) in porcine muscle and 52.8-112.4% (RSDs 2.3-16.9%) in chicken muscle. The limits of detection (LODs) and limits of quantification (LOQs) were 2-32 and $7-96\;{\mu}g/kg$ in porcine muscle, and 4-32 and $13-97\;{\mu}g/kg$ in chicken muscle, respectively. These values were lower than the maximum residue limits (MRLs) established by the European Union. The sum of all SAs residues present should be less than $100\;{\mu}g/kg$.

• Korean Journal of Veterinary Service
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• v.20 no.1
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• pp.79-93
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• 1997

The sulfonamide is one of potentiative antimicrobial agents which is being used widely in veterinary medicine for control of several animal diseases such as mastitis as well as for promotion of growth. However, the misusages of sulfonamides in food producing animals, especially cattle produce several considerable problems in human health caused from residues of this antibiotic in milk product. To determine the most effective analytical methods for residual sulfonamides in raw milk, this study was performed comparatively using by some applicable screening detecting method such as TTC, Charm II test (sulfonamides), and Lactek tests (sulfamethazine kit). The positive result from screening tests was confirmed by HPLC method. Milk samples (540 raw milks) were collected from dairy farms. Results of this study are summariezed as follorrs ; 1. All samples (540 raw milks) showed negative response from TTC test, however, 18 raw milks of those samples responded positively to Charm II test. 2. By Lactek test, residual sulfamethazine was detected from 4 raw milks. Fifteen raw milks of 18 samples which were classified as positive one by Charm II test, showed positive response 3. Retention time of sulfonamides added at the level of 100ppb into sklm milk was ranged from 1.55 minute to 23.3 minute. Recovery rates of sulfonamides were variable from 6.7% upto 94.2% depended on the types of sulfonamlde. 4. Single type of sulfonamides was detected from 10 raw milk samples, 2 types of sulfonamides from 3 samples and 3 types from 2 raw milks by HPLC. 5. Sulfonamides was detected in this study were 5 types : 11 samples for sulfisomidine, 5 samples for sulfamethazine, 3 samples for sulfadlmethoxine, 2 samples for sulfathiazole and 1 sample for sulfadiazine. 6. The highest levels of residual sulfonamides was 210.3 ppb of sulfamethazine but the lowest concentration of residue was 2.2 ppb of sulfamethazine and sulfisomidine, respectively. Number of samples detected positively in this experiment were belows : above 100 ppb for 1 sample (4.5%) (sulfamethazine), 50~100 ppb for 4 samples (18.1%) (each 2 samples for sulfamethazine and sulfisomidine, respectively), 25~50 ppb for 6 samples (27.1%) (2 sulfisomidine, each 1 sample for sulfadiazine, sulfadimethoxine, sulfamethazine and sulfathiazole, respectively), 10~25ppb for 3 samples (13.7%) (3 sulfisomidine), and below 10ppb for 8 samples (36.4%) (4 sulfisomidine, 2 sulfadimethoxine and each 1 for sulfamethazine and sulfathiazole).

• 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.

• Korean Journal of Veterinary Research
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• v.46 no.4
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• pp.295-304
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• 2006

Residual materials such as veterinary drugs, environmental contaminants, and pesticides are affecting food safety. High resolution techniques and quality controls are needed to analyze these materials from part per million to part per trillion quantities in food. In order to achieve quality results, standardized methods and techniques are required. Our laboratories were prepared to obtain a certificate of accreditation for ISO/IEC 17025 in the analytical criteria of animal drugs, dioxins, pesticides, and heavy metals. ISO together with IEC has built a strategic partnership with the World Trade Organization with the common goal of promoting a free and fair global trading system. ISO collaborates with the United Nations Organization and its specialized agencies and commissions, particularly those involved in the harmonization of regulations and public policies including the World Health Organization and CODEX Alimentarius for food safety measurement, management and traceability. Our goal was to have high quality analysts, proper analytical methods, good laboratory facilities, and safety systems within guidelines of ISO/IEC 17025. All staff members took requirement exams. We applied proficiency tests in the analysis of veterinary drugs (nitrofuran metabolites, sulfonamide and tetracyclines), dioxins, organophosphorus pesticides, and heavy metals (Cd, Pb, As) to the Food Analysis Performance Assessment Scheme (FAPAS) at Central Science Laboratory, Department for Environment Food and Rural Affairs (DEFRA), England. The results were very satisfactory. All documents were prepared, including system management, laboratory management, standard operational procedures for testing, reporting, and more. The criteria encompassed the requirements of ISO/IEC 17025:1999. Finally, the Korea Laboratory Accreditation Scheme (KOLAS) accredited our testing laboratories in accordance with the provisions of Article 23 of the National Standards Act. The accreditation will give us the benefit of becoming a regional reference laboratory in Asia.