• 한국식품위생안전성학회지
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• 제9권1호
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• pp.37-42
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• 1994

Four sulfoanmides ; sulfamerazine ; sulfamethazine, sulfathiazole and sulfadimethoxine from muscle, kindney, liver and heart tissues of pork and chicken by LC. Residual sulfonamides were extracted with dichloromethane and determined on a Sperisorb ODS-1 column(250mm$\times$4.6mm id) with acetonitrile/water/acetic acid (30/70/0.3 v/v) as a mobile phase at 260nm. Recoveries from 4 tissues of pork and chicken samples fortified with 50 and 100 ppb were 71.2~87.2% and 73.7~89.6%, respectively. The detection limit was 0.03 $\mu\textrm{g}$/g in each drug. Sulfamethazine in 5 samples of pork. And sulfadimethoxine in 5 samples and sulfamethazine in 3 samples were also detected from 41 samples of chicken. The order of residue levels of sulfonamides in tissues was kidney>liver>heart>muscle, respectively. The residue levels of sulfonamides from kidney and liver were 0.03~0.15 $\mu\textrm{g}$/g in porks and 0.03~0.10 $\mu\textrm{g}$/g in chickens.

• 한국동물위생학회지
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• 제16권1호
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• pp.11-19
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• 1993

This experiment was carried out to detect the residues of sulfonamides in raw milk. Raw milks which does not contain sulfonamides was collected from one of the farm and fortified with 5 sulfonamides (sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfadimethoxine, sulfaqinoxaline). The sulfonamides in the fortified sample were extracted and detected by High Performance Liquid Chromatography. UV /vis detector was used in this experiment. The results obtained were summarized as follows : 1. Chloroform was good as a extracting solution. 2. 15.5% methanol in PDP as a mobile phase solution was best detective condition for SMR, SMT, SMM. But for SDM and SQN the best condition was 23% methanol. 3. The detectable limits of SMR, SMT, SMM were 2ppb. but SDM and SQN were 20ppb because of delayed retention time and relatively low recovery rate. 4. The peaks of SMR, SMT, SMM and SDM were erected at baseline and the apexes were sharp but SQN was round shape.

• 한국응용약물학회:학술대회논문집
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• 한국응용약물학회 1996년도 춘계학술대회
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• pp.176-176
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• 1996

축산식품중에 잔류하고 있는 sulfamethazine을 검출하기 위하여 sulfamethazine에 대한 단클론항체를 생산하고 이를 이용하여 효소면역측정법을 개발하였다. 면역원은 sulfamethazine에 KLH를 그리고 흡착항원은 BSA를 glutaraldehyde법으로 결합시켰다. 면역원으로 Balb/c mouse를 면역시킨 다음 비장 형질세포률 얻어 myeloma cell과 융합하여 융합잡종세포를 만들었다. Sulfamethazine에 대한 항체를 분비하는 융합잡종세포를 단계회석법과 ELISA를 이용하여 cloning하여 D2, A9, B8, Bl 클론을 얻었다. 이들 클론에서 얻어진 단클론항체를 사용하여 indirect competitive ELISA를 실시하여 표준곡선을 작성하여 본 결과 농도의존성 곡선을 얻을 수 있었다. 4클론중에서 A9 클론을 사용하여 다른 유사한 sulfonamide듣과 p-aminobenzoic acid와 교차반응을 조사한 결과 sulfamerazine에 12.5%의 교차반응을 보였으나 다른 설파제에 대해서는 교차 반응을 보이지 않았다.

• 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.

• 분석과학
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• 제23권5호
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• pp.437-445
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• 2010

본 연구에서는 동물용 의약품으로 널리 사용되고 환경 중 잔류 가능성이 높은 설폰아미드계 항생제 5종 (sulfadiazine, sulfamerazine, sulfamethazine, sulfamethoxazole, sulfathiazole) 및 대사체 5종($N^4$-acetylsulfadiazine, $N^4$-acetylsulfamerazine, $N^4$--acetylsulfamethazine, N4-acetylsulfamethoxazole, sulfamethoxazole-$N^1$-glucuronide)의 분석방법을 연구하였다. 다양한 전처리 조건을 비교 검토하여 최적의 동시 추출방법과 LC/ESI-MS/MS를 이용한 기기분석 조건을 확립하였다. 카트리지별 추출효율은 C18 카트리지에서 12~94%, HLB 카트리지에서 60-95%, MCX 카트리지에서 25-123%였으며, MCX와 HLB 카트리지를 결합한 방법의 회수율은 70-90%이었다. HLB를 선택하여 확립된 분석방법의 회수율은 66~115%, 상대표준편차 5~17%이었으며, 방법검출한계는 0.001~0.187 ng/mL 였다. 이를 실제 환경시료에 적용한 결과 4종의 설폰아미드 항생제가 0.008~2.153 ng/mL 농도범위로 검출되었으며, 대사체의 경우 $N^4$-acetylsulfamethoxazole이 확인되었으나 검출한계 미만으로 관찰되었다.

• 대한수의학회지
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• 제30권1호
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• pp.41-49
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• 1990

These experiments were carried out to develop a novel, simple, and rapid method to determine urinary sulfonamides using fluorescamine by spectrofluorometry. To get optimal conditions for the sulfonamide-fluorescamine reaction, sulfonamides such as sulfamethazine, sulfamerazine, sulfadimethoxine and sulfamonomethoxine, dissolved in buffers with various pH ranges were reacted with various concentrations of fluorescamine. and then, the fluorescence intensity and stability of the fluorophore were measured. To eliminate the interfering substances in urine, the fluorophore in buffers and urine with a definite pH range was extracted with some organic solvents. After then the fluorescence intensity was measured in organic and aquous phases. The results obtained were summarized as follows: 1. The maximal fluorescence of sulfonamides was presented in acidic state, pH 4.5~5.0, at 30 minutes after reaction. 2. The optimal concentration ratio of sulfamethazine and ffuorescamine was more than 1 : 40 in mole. 3. In pH 4.0, the intensity was maximal but was time-dependent, whereas in pH 8.0, the intensity was time-independent. 4. Sulfamethazine-fluorescamine conjugate could be dissolved in some of organic solvents in acidic state such as chloroform, n-butanol, and ethylacetate. 5. Sulfamethazine-flnorescamine conjugate in swine urine coule be extracted with ethylacetate in acidic state, pH 4.0~5.0.

• 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.

• 한국동물위생학회지
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• 제29권3호
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• pp.331-338
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• 2006

This survey was carried out to detect the residual antibiotics in beef (n = 1,071), pork (n=7,837) and chicken (n=1,536) from slaughter houses in Gyeongbuk province by EEC-4 plate method, Charm II and HPLC during 2005. Residues of antibiotic were detected from 9 beef (0.8%) and 119pork (1.52%) by EEC-4 plate method, and total positive rates were 1.23% (128). 126 samples of the 128 positive samples by the EEC-4 plate method were detected by charm II test. 128 samples were classified as tetracyclines 110 (95.5%), ${\beta}$-lactam 2 (1.6%), sulfonamide 22 (17.2%), quinolone 1 (0.8%). The highest residual concentration of oxytetracycline, tetracycline, chlor-tetracycline, penicillin, sulfamethazine, sulfadimethoxine, sulfaquinoxaline, sulfamerazine, sulfamonomethoxine and enrofloxacin were 7.57, 0.27, 0.40, 0.24, 14.24, 4.33, 8.59, 0.12, 0.09 and 1.98 ppm, respectively and 49 samples were exceeded legal admitted levels.

• 한국동물위생학회지
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• 제27권3호
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• pp.265-272
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• 2004

It was carried out to compare the residual materials by EEC 4-plate, Charm II and HPLC method in the muscles of cattle and pigs from slaughter-houses in Seoul from 2000 to 2003. Residual materials were detected from $1.10\%$(73/6,623) samples by EEC 4-plate method, and $10.93\%$(55/503) samples by Charm II method. The highest residual concentration(ppm) of oxytetracycline, tetracycline, chloramphenicol, chlortetracycline, sulfamethazine, sulfamerazine, sulfadimethoxine, penicillin and sulfamonomethoxine were 25.5, 3.46, 3.26, 1.5, 0.3, 0.2, 0.2, 0.14, and 0.07, respectively. Eighty nine samples were classified as 58($65.17\%$) only tetracyclines, 20($22.47\%$) only sulfonamides, 3($3.37\%$) only ${\beta}$-lactams, 2($2.25\%$) only chloramphenicol, 4($4.49\%$) tetracyclines and sulfonamides simultaneously, 1($1.12\%$) chloramphenicol and sulfonamides simultaneously, and 1($1.12\%$) chloramphenicol, sulfonamides and tetracyclines simultaneously.

• 한국동물위생학회지
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• 제21권4호
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• pp.379-383
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• 1998

This survey was carried out to determine 5 residual sulfonamides(sulfamerazine : SMR, sulfamethazine : SMT, sulfamonomethoxine : SMM:, sulfadimethoxine : SDM, sulfaquinoxaline : SQX) in muscle of mouse. For this investigation, pertaining detection wavelength, residual levels and residual times in muscle of mouse were summarized as follows ; 1. Pertaining detection wavelength of 5 residual sulfonamides(SMR, SMT, SMM, SDM, SQX) was 270nm by HPLC/UV detection. 2. After 1 day put a stop to sulfonamides administration, residual levels was 1∼l.5ppm, but were not detected at day 7 3. Withdrawal time of 5 sulfonamides were about 7 days suspectly.