• 한국식품위생안전성학회지
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• 제12권2호
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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.

• 대한수의학회지
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• 제34권4호
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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.

• 한국동물위생학회지
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• 제19권1호
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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.

• 농업과학연구
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• 제12권2호
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• pp.349-355
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• 1985

가금질병(家禽疾病)의 예방(豫防) 및 치료(治療) 그리고 성장(成長) 및 비육촉진(肥育促進)의 목적(目的)으로 급여(扱與)한 sulfonamides의 계육(鷄肉) 및 계란내(鷄卵內) 잔류(殘留)할 가능성(可能性)이 주목(注目)됨으로 그 이행잔류상(移行殘留狀)을 구명(究明)함으로써 식육내(食肉內)의 허용직(許容直) 설족(設足), 투약법(投樂法)의 개선(改善) 그리고 식품위생산(食品衛生上)의 공해(公害)를 방지(防止)할 수 있을 것으로 생각되어 실시(實施)한 실험결과(實驗結果)를 요약(要約)하면 다음과같다. 1. Bacillus subtilis 균(菌)은 Sulfonamides에 대(對)하여 감수성(減受性)이 예민(銳敏)하여 0.05ppm까지 검출(檢出)할 수 있었다. 2. 혈액내(血液內) 잔류상(殘留狀)은 1회(回) 투약후(投藥後)에는 48시간(時間)까지 검출(檢出)할 수 있었고, 3회(回) 투약(投藥)한 구(區)에서는 3구(區) 모두 최종투약후(最終投藥後) 60시간(時間)까지 검출(檢出)할 수 있었다. 3. 각(各) 장기조직내(臟器組織內)에서는 3구(區) 다같이 최종투약후(最終投藥後) 5일(日)까지는 검출(檢出)할 수 있었으나 10일(日)에서는 담즙(膽汁)을 제외(除外)하고는 모두 검출(檢出)할 수 없었다. 4. 계란(鷄卵)의 난백(卵白)에서는 최종투약후(最終投藥後) 3구(區) 모두 5일(日)까지는 검출(檢出)이 가능(可能)하였으나 난황(卵黃)에서는 3구(區) 모두 5일(日)에서 흔적(痕迹)만 남기고 검출(檢出)할 수 없었다. 5. 담즙내(膽汁內)의 잔류(殘留) 유무(有無)는 각(各) 장기조직(臟器組織) 및 계란(鷄卵)의 식용(食用) 여부(與否)를 판정(判定)하는데 좋은 측도(測度)가 될 수 있을 것이다.

• 한국동물위생학회지
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• 제21권1호
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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.

• 대한수의학회지
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• 제34권1호
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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.

• 한국식품과학회지
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• 제26권3호
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• pp.221-225
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• 1994

1992년 6월부터 1993년 6월에 걸쳐 본원에 의뢰된 전라남도 내에서 유통된 쇠고기 30건, 닭고기 15건과 도축장에서 임의로 채취한 돼지고기 10건, 돼지신장 10건에 대해 HPLC법을 이용하여 설파제 잔류농도와 회수율을 분석하였다. 식육중 설파제 첨가 회수율은 sulfamerazine 71.7%, sulfamethazine 80.3%, sulfamonomethoxine 71.6%, sulfadimethoxine 70.9, sulfaquinoxaline 68.4%로 나타났으며 설파제 첨가 농도에 따른 회수율의 차이는 보이지 않았다. 총 65건중 국내잔류허용 기준치인 0.1 ppm을 초과한 경우는 한건도 없었으며, 일본 허용기준치인 0.005 ppm을 초과한 경우는 닭고기 2건(sulfamerazine 0.077 ppm, sulfamethazine 0.075 ppm)과 돼지신장 1건(sulfadimethoxine 0.052 ppm)으로 총 3건(4.6%)이었으며, 돼지고기에서는 검출되지 않았거나 극미량(<0.005 ppm) 검출된 경우라도 신장에서는 고기에서보다 높은 농도로 검출되어 고기보다 신장의 잔류농도가 높음을 알 수 있었다.

• 한국환경농학회지
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• 제28권3호
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• pp.266-273
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• 2009

HPLC를 이용한 분석은 항균, 항생제의 정량분석에 있어 가장 널리 이용되고 있으며, 최근에 개발된 MSPD방법은 고정상을 직접 갈아서 추출, 정제하는 방법으로 전처리 시 그조작이 간단하며, 유기용매가 적게 들고 전처리 시간이 짧다는 장점이 있다. 본 연구는 HPLC와 MSPD방법을 이용하여 가축 중 소비량이 가장 많은 돼지고기와 생선 중 회로 가장 많이 소비되는 광어에 대하여, 식품 중 잔류 가능성이 높은 tetracycline계 항생제 3종(oxytetracycline, tetracycline, chlortetracycline)과 sulfonamide(sulfadimethoxine, sulfamerazine, sulfamethazine, slfaquinoxaline, sulfamonomethoxine) 5종의 동시분석방법을 개발코자 하였다. HPLC의 최적 분석조건으로 파장은 tetracycline계 항생물질은 360 nm에서 sulfonamide는 270 nm였으며, 이동상은 TC와 SMR이 분리되는 시점인 15분까지는 pH 4.5, oxalic acid : acetonitrile (78.5 : 21.5, v/v)로 분석하고 이후 30분까지는 pH 6.1, oxalic acid : acetonitrile (78.5 : 21.5, v/v)로 분석을 실시하였을 때 기존의 실험방법보다 피크의 분리도와 검출한계의 개선이 이루어졌으며 이를 토대로 8가지 성분의 MRLs인 $0.1{\sim}0.2mg{\cdot}kg^{-1}$까지 충분히 분석이 가능하였다. MSPD 적용을 위한 시료의 전처리 방법개선은 기존의 0.5 g으로 제한된 시료량을 3 g으로 늘릴 수 있었고 dichloromethane 20 mL와 methanol 20 mL로 연속적으로 8가지 성분을 동시에 용출시켜 sulfonamide는 $80.25{\sim}101.25%$, tetracycline계 항생물질은 $85.77{\sim}121.42%$의 회수율을 얻을 수 있었다.

• Food Science and Biotechnology
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• 제18권6호
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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 $100\;{\mu}g/kg$.

• 대한수의학회지
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• 제40권3호
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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%.