• Journal of Food Hygiene and Safety
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• v.12 no.2
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• pp.117-124
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• 1997

A simple, rapid and simultaneous analytical method is described for the detection of Sulfonamide and Tetracycline residues, i.e., Sulfamerazine (SMR), Sulfamethazine (SMT), Sulfamonomethoxine (SMM), Sulfadimethoxine (SDM), Sulfaquinoxaline (SQN), Oxytetracycline (OXY), Tetracycline (TC), Chlortetracycline (CTC). Blank control and sulfonamide and tetracycline fortified fish muscle samples (0.5 f) were blended with octadecylsilyl (C18, 40 ${\mu}{\textrm}{m}$, 21% load, 60$\AA$) derivatized silica packing material (2 g). Blended fish samples were washed with hexane, then, benzene and dichloromethace were used for the elution of tetracycline and sulfonamide were analyzed by HPLC. Correlation coefficients of standard curves for individual sulfonamide and tetracycline isolated from fortified samples were linear (0.9993$\pm$0.0003~0.9997$\pm$0.0003, 0.9493$\pm$0.078~0.9753$\pm$0.036), respectively. The average percentage recoveries of sulfonamide and tetracycline ranged as 80.86~96.52% to 85.88~92.23%, and 30.01~37.12% to 65.89~73.40%, for the concentration range (0.1~1.0 ppm) examined, respectively. Limit of detection for sulfonamide was 0.0012 ppm for SMR in Paralichthys Olivacleus and 0.0020 ppm for SMR, 0.015 ppm for SMM in Cyprinus Carpio. The applicability of this procedure is demonstrated by separation and detection of incurred tetracycline and sulfonamide residues in fish muscle tissue.

• Korean Journal of Veterinary Research
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• v.34 no.4
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• pp.843-850
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• 1994

The study was carried out to determine the residues of sulfonamides in swine edible tissues with high performance thin layer chromatography. For this purpose, the Rf values of sulfonamides in various solvent systems and the recovery rate of sulfameathazine from sampike saples were obtained. Thirty-four samples collected from meat market in Seoul were analyzed. The results obtained from the present study were followings: 1. The average recovery rate of sulfamathazine residues from spiked tissues 0.05, 0.1, 0.5 and 1mg/kg sample weight was 85%. 2. Two of 34 samples of pork for domestic consumption were reported to have been exceeded 0.05 ppm in sulfamethazine residues degree. 3. On the basis of the results, the degree of residues of sulfamethazine in swine meat for domestic consumption is seemed not to be dangerous for public health.

• Korean Journal of Veterinary Service
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• v.19 no.1
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• pp.39-45
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• 1996

Sulfonamides are widely used to treat mastitis of cattle in field. The study was carried out to analyze sulfonamid residues In raw milk from south Kyeonggi area. The milk sample was deproteinated with acetone and defatted with hexane. The residual sulfonamides were extracted with ethylacetate, concentrated under vaccum, reconstituted with the acetate buffer-methanol mixture, reacted with fluorescamine, and then analyzed by HPLC-fluorescence detector(EX. 39nm, Em. 495nm) with methanol : acetate buffer system(3/2, v /v) as a mobile phase. The results analyzed by Thin layer chromatography and High performance liquid chromatography were summarized as follows. 1. A total of 24 cases out of 478 raw milk samples(5.0%) collected during April and May showed positive reaction to sulfonamide residues. Among 24 positive reactors, 9 cases were positive to sulfanilamides(32.1%), 8 cases were positive to sulfathiazoles(28.6%) and 5 cases were positive to sulfamonomthoxines (7.9%) , respectively. 2. During July and August, 31 cases out of 464 raw milk samples(6.7%) showed positive re action to sulfonamide residues. Among them S cases were positive to sulfanilamides, 5 cases sulfathiazoles and 5 cases sulfamonomethoxines(16.1%), respectively.

• Korean Journal of Agricultural Science
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• v.12 no.2
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• pp.349-355
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• 1985

The effects of sulfadimethoxine administration on the residues in tissues and eggs were examined in Laying Hens. Sulfadimethoxine was administered orally to White Leghorns at a excessive dose level (300 mg/kg/day), therapeutic dose level (150mg/kg/day) and prophylactic dose level (50mg/kg/day). Sulfonamide residues were measured in blood, tissues (muscle, liver, kidney, lung and bile) and eggs (egg whites and egg yalks) with paper disc methods. The results obtained were summarized as follows: 1. Bacillus subtilis was very susceptible to sulfonamide, and detectable to the level of 0.5 ppm. 2. In blood serum levels, it was detectable until 48 hours post-treatment in once administration of therapeutic dose level, and also detectable until 60 hours post-treatment in all groups of three times administration with excessive, therapeutic and prophylactic doses. 3. As for the tissues residues, sulfonamides were detectable until 5 days post-treatment in muscle, liver, kidney, lung and bile of all groups, but were not detectable except bile on 10 days of post-treatment. 4. Sulfonamide residues in egg whites of all groups were detectable until 5 days, but in egg of all groups were not detectable but trace amounts at 5 days post-treatment. 5. The presence or absence of sulfonamide in bile may be standard to judge the edibility of organ tissues and eggs.

• Korean Journal of Veterinary Service
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• v.21 no.1
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• pp.13-20
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• 1998

This survey was carried out to detect the residual antibiotics and sulfonamides in emergency slaughtered cattle(n=265) from slaughter houses in Kyeonggi province by EEC 4-plates method, Charm II and HPLC. The results were summarized as follows ; 1. Antimicrobial substances were detected from 24 samples(9.1%) by EEC 4-plates method and the detection ratio were highest in summer(13.8%). 2. Twenty-two of the 24 positive samples were classified as sulfonamide(34.4%), TCs(31.3%), $\beta$-lactam(23.5%) and aminoglycoside(9.3%) by Charm II test. 13(59.1%) of the 22 samples contained single agent and 9 samples(40.9%) contained 2 or more agents. 3. Oxytetracycline(27.3%), penicillin G (27.3%) and sulfathiazole(18.2%) were detected in 20 from 22 samples by the HPLC and Charm II test. 4. The residual concentration of oxytetracycline, penicillin G and sulfonamide were 0.29~9.30 ppm, 0.05~9.58 ppm and 0.04~7.59 ppm, respectively and 19 samples(7.2%) were exceeded tolerance levels.

• Korean Journal of Veterinary Research
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• v.34 no.1
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• pp.141-146
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• 1994

돈육의 가열과 냉동저장시 잔류된 설폰아미드가 증가 또는 감소되는 정도를 조사하였다. 설파메라진, 설파메타진, 설파모노메톡신, 설파디메톡신, 설파퀴녹사린을 돈육에 100ng/g씩 주사하고 30분간 $60^{\circ}C$로 가열하였을 때 설파메타진은 40%증가하였으나, $60-120^{\circ}C$로 가열한 다른 설폰아미드는 12-22% 감소하였다. 4주간 $-20{^{\circ}C}$이하로 냉동하였을 때, 설파메라진과 설파퀴녹사린은 각각 12%, 19% 감소하였으나 다른 설폰아미드는 변화가 없었다. 설폰아미드의 검출한계는 고상분산을 이용한 정제시 2.6-27ng/g이있으며, 액상분배를 이용한 정제시 25-36ng/g이었다. 본 실험의 결과 돈육중의 설폰아미드는 가열과 냉동저장에 따라 안정성이 변화될 수 있으며, 잔류물 정제방법으로는 고상분산과 액상분배방법을 이용할 수 있을 것으로 생각된다.

• 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.

• Korean Journal of Environmental Agriculture
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• v.28 no.3
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• pp.266-273
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• 2009

This study was conducted to develop more convenient simultaneous determination method by matrix solid phase dispersion (MSPD) and HPLC for sulfonamides such as sulfamerazine (SMR), sulfamethazine (SMT), sulfamonomethoxine (SMM), sulfadimethoxine (SDM), sulfaquinoxaline (SQX), and tetracyclines including oxytetracycline (OTC), tetracycline (TC) chlortetracycline (CTC) in prok and flatfish. The limits of detection were 0.047 $mg{\cdot}kg^{-1}$ for OTC, TC, SMR, SMT and SMM, and 0.033 $mg{\cdot}kg^{-1}$ for CTC, SDM, and SQX, respectively. So it is sufficiently possible to detect the eight tetracyclines and sulfonamides under their MRLs ($0.1{\sim}0.2mg{\cdot}kg^{-1}$). The average percentage recoveries of sulfonamides and tetracyclines from pig muscle and flatfish spiked standard solution were approximately $80.25{\sim}101.25%$ and $85.77{\sim}121.42%$, respectively. Therefore this method was efficient for simultaneous analysis of eight tetracyclines and sulfonamides.

• 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 Research
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• v.40 no.3
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• pp.601-609
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• 2000

An enzyme linked immunosorbent assay (ELISA) was developed to screen residues of sulfadimethoxine (SDM) in edible animal products. An indirect competitive ELISA was allowed to compete with rabbit anti-SDM for binding to a limited amount of SDM-gelatin conjugate and SDM in serum samples. Sera was diluted 20 times with phosphate buffered saline (PBS) and boiled for 5 minutes to destruct immunoglobulins of serum. Detection limit of this competitive ELISA for SDM was 0.1 ppb or less. Among eight sulfonamide analogues tested for specifity, only sulfamonomethoxine showed significant cross-reaction in the assay. The EC-50 value for sulfamonomethoxine was 3.5 ppm. Recovery of SDM in spiked serum samples between 100 ppb and 500 ppb ranged from 110.7% to 128.9%.