• 한국동물위생학회지
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• 제27권1호
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• pp.17-29
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• 2004

A multiresidual analysis was performed to determine 12 sulfonamides(sulfacetamide, sulfadiazine, sulfisomidine, sulfathiazole, sulfapyridine, sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfisoxazole, sulfamethoxazole, sulfaquinoxaline, and sulfadimethoxine) in beef and pork simultaneously. The multiresidual analysis for the sulfonamides currently used was able to analyze 5 kinds of sulfonamides at the same time. The method of this 12 sulfonamides multiresidual analysis in this study was matrix solid-phase dispersion(MSPD) by high performance liquid chromatography (HPLC) and liquid chromatography mass spectrometry (LC/MS). The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM: Ethylacetate(3:1), DCM:EA(9:1). Also, samples (84 beef and 205 pork samples) which were positive by EEC-4 plate test from 2001 to 2003 were tested to investigate the kinds of sulfonamides using HPLC. The results from the study were as follows; 1. The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM:Ethylacetate(3:1), DCM:EA(9:1). The method of extraction solvent with DCM:ethyl acetate(9:1) was the most excellent(87.7∼99.3%) in separation and reappearance. 2. In the LC/MS analysis. of sulfonamides, signal to noise ratio was showed relatively high in the positive mode and special ion in the quality analysis was determined via [M+H]$\^$+/ and m/z 156. A spectrum of sulfonamides was showed from all 12 sulfonamides. 3. The samples positive by the EEC-4 plate, a screening test method, were categorized by sulfonamides through Charm II and confirmed the kinds of sulfonamides through HPLC. 1) Among 84 beef samples positive by EEC-4 plate, 20 samples were positive by Charm II and identified as 7 sulfamethazine, 9 sulfadimethoxine, 1 sulfamonomethoxine and 3 unknown status. 2) Among 205 pork samples positive by EEC-4 plate, 42 samples were positive by Charm II and identified as 19 sulfamethazine, 1 sulfadimethoxine, 4 sulfamonomethoxine and 5 unknown status.

• 한국동물위생학회지
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• 제20권4호
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• pp.339-348
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• 1997

The purpose of the survey were determined the residual antibiotics and tetracyclines in beef(n=1,364), pork(n=2,817) and chickens(n=1,921) by the EEC 4-plate method, Charm IIand HPLC. The results were summarized as follows ; 1. The recovery rates in spiked samples were 98.8-107.2% for oxytetracycline(OTC), 33.2-48.6% for tetracycline(TC) and 64.1-72.3% for chlortetracycline(CTC) at 0.05-0.1ppm by HPLC using MSPD. 2. Residues of antibiotic were detected from 10 beef(0.75%) and 36 pork(1.31%) by EEC 4-plate method. In case of chickens were not detected. 3. Twenty-eight from 46 positive samples by the EEC 4-plate method were classified as TCs(60.9 %) by Charm II and TC of 12 samples were detected by HPLC. 4. Ten samples were detected levels of OTC ranging from 0.035 to 0.635 ppm and 3 samples were levels of CTC ranging from 0.066 to 0.150 ppm. OTC and CTC levels in 3 beef and 4 pork samples were exceeded the current tolerance level of 0.1 ppm.

• 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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• 제25권3호
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• pp.285-294
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• 2002

The present studies were carried out to determine antibiotics residues in pork and beef muscles by EEC-4-plate and HPLC. A total of 2,534 samples of pork muscles and 1,070 samples of beef muscles from slaughter houses were collected in Gyeongnam area from January to December, 2001. The results were summarized as follows; 1. Recovery rates of TCs, Sulfa drug, Penicillin G from fortified pork and beef muscles ranged as 68.79～98.24%, 78.21～94.58% and penicillin G 63.35～67.24% respectively, by HPLC. 2. Antibiotics residues were detected in 36 sample(1.42%) of pork muscles, 29 sample (2.71%) of beef muscles by EEC-4-plate. 3. Detection rate of antibiotic residues 14 samples(0.55%) and 26 samples(2.43%), in pork and beef muscles, respectively by HPLC. Concentration of residues in 22 sample(2.06%) of beef muscle were higher than tolerance level in korea. 4. Antibiotics detected were sulfamethazine(47.37%), tetracycline(15.79%), oxytetracycline (15.79%), penicillin G(15.79%), sulfamerazine(5.26%) in pork muscle samples and oxyteracycline (37.21%), penicillin G(30.23%), sulfamethazine(20.93%), tetracycline(4.65%), sulfamerazine (2.33%), sulfadimethoxine(2.33%), sulfaquinoxine(2.33%) in beef muscle samples.

• 한국동물위생학회지
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• 제26권2호
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• pp.113-119
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• 2003

This study was carried out to compare the antibiotic residues in the muscles of cattle and pigs from slaughter-houses in Seoul from 2000 to 2002 by EEC-4-plate, Charm II and HPLC methods. The results were summarized as follows; 1. Residual materials were detected from 41 samples(0.6%) by EEC-4-plate method from random sampling and 38 samples(12%) by Charm II method from directed sampling. 2. Violation rates were 0.3% by monitoring and 4.7% by surveillance program. 3. The 35 samples were classified as tetracyclines 30(86%), sulfonamides 4(11%), ${\beta}$-lactams 1(3%) and two samples simultaneously determined oxyteracycline plus sulfadimetoxine, and sulfamerazine plus sulfadimetoxine. 4. The highest residual concentration(ppm) of chlortetracycline, oxytetracyline, sulfamethazine, sufadimetoxine and penicillin were 0.5, 12.0, 6.4, 2.6 and 0.44, respectively.

• 한국동물위생학회지
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• 제15권2호
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• pp.93-100
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• 1992

The purpose of the present survey was to evaluate the antibiotic residues in meats and internal organs such as muscle, liver, heart, kidney and spleen of cattle (n=59) and pigs (n=115). The EEC-4-plate-method were employed. The results were obtained as follows ; 1. In BS 6.0, BS 7.2 and BS 8.0 used as media to detect antibiotic residues, the zone($M{\pm}SD,$ cm) of bacterial growth inhibition was narrow($1.40{\pm}0$) in meats, whereas the zone was wide($1.69{\pm}0.25-1.88{\pm}0.23$ and $1.58{\pm}0.18-1.86{\pm}0.15$ in cattle and pigs, respectively) in internal organs. But in SL 8.0, it was difficult to detect the zones ($0-1.40{\pm}0$) of both meats and internal organs. 2. Residues of antibiotic in beef and pork were rarely detected in BS 6.0, BS 7.2 and BS 8.0 (range 1.7-11.9% and 2.6-4.3%, respectively), whereas residual percentages of internal organs were relatively higher(range 69.5-96.6% and 43.5-84.3%, respectively). But in SL 8.0, it was not detected in both beef or pork, whereas they were 0-13.6% and 0-4.3% in interanal organs.

• 한국어병학회지
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• 제11권1호
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• pp.77-81
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• 1998

실험에는 Bacillus subtilis BGA, Bacillus cereus var. mycoides ATCC 11778, Micrococcus luteus ATCC 9341을 상법에 따라 제작하여 muller hinton agar(Difco)에 각각 접종한 뒤, 3가지 조건의 pH가 조정된 검사용 평판배지(plate)인 B. subtilis(pH 6.0), B. cereus(pH 6.0), B. subtilis(pH7.2), B. subtilis(pH 8.0), M. luteus(pH 8.0)의 EEC 4-plate변법을 이용하였다. 넙치에 옥시테트라싸이클린(OTC)을 농도 100 mg/kg/day으로 단 1회 강제 경구 투여한 후 1일, 3일, 5일, 10일, 15일, 20일, 25일 30일마다 3마리씩 채취하여 시료의 처리를 각각 달리한 근육직접법, 추출디스크법, 직접디스크법의 3종류 간이스크리닝법으로써 OTC의 잔존유무를 분석하였다 B. subtilis(pH 6.0)배지는 투여 후 1일째 근육직접법에서만 양성반응으로 의심되는 의양성 반응(${\pm}$)을 나타내었을 뿐 30일까지 간이스크리닝법 3종류가 모두 음성 반응을 나타내었다. B. subtilis(7.2), B. subtilis(8.0), M. luteus(8.0)배지는 투여 후 1일째부터 30일까지 간이스크리닝법 3종류가 모두 음성반응을 나타내었다. 그러나 B. cereus(pH 6.0)배지는 1일째부터 15일까지 간이스크리닝법 3종류가 모두 명확한 양성반응, 투여 후 20일째 근육직접법과 직접디스크법은 의양성반응(${\pm}$)을 보였으나 추출디스크법은 분명한 음성반응, 그리고 투여 후 25일째 및 30일째는 시험조작법 모두가 음성반응을 나타내었다. 따라서 근육직접법, 추출디스크법, 직접디스크법의 간이스크리닝법 3종류는 OTC의 양성반응 판정에 커다란 차이가 없었으며, B. cereus는 OTC의 모니터링에 유효한 균주라는 사실을 확인하였다.

• 한국식품위생안전성학회지
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• 제19권1호
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• pp.12-18
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• 2004

1. 닭고기에서 4종의 플루오로퀴놀론계 합성항균제(ofloxacin, norfloxacin, ciprofloxacin, enrofloxacin)를 액상추출법으로 추출하여 형광검출기와 HPLC를 이용하여 동시 정량 분석하는 방법을 확립하였으며 분석조건으로서 컬럼은 Symmetry Cl8(250${\times}$4.6 mm id, 5 $\mu\textrm{m}$), 이동상은 0.4% triethylamine 및 0.4% phospholic acid 수용액, methanol 및 acetonitrile 혼합용액(800: 100: 100, v/v/v)을 사용하였으며, 형광검출기는 여기파장 278 nm, 측정파장 456 nm으로 그리고 유속은 1.0 $m\ell$/min., 주입량은 50 ${\mu}\ell$로 하였다. 확립된 분석조건으로 측정한 ofloxacin, norfloxacin, ciprofloxacin, enrofloxacin 표준품의 표준곡선식에서 모두 상관계수 0.999이상의 양호한 직선성을 보였으며, 첨가한 닭고기의 크로마토그람에서도 각각의 물질별 분리시간대에 방해 피크 없이 양호한 분리도를 나타내었다. 0.05∼0.2 $\mu\textrm{g}$/g 첨가한 시료에서 평균 회수율은 ofloxacin 92.0∼95.4%, norflokacin 84.2∼87.3%, ciprofloxacin 78.3∼82.2%, enrofloxacin 91.3∼95.3%이었으며 변이계수(CV)는 2.7∼9.4%이었다. 4종의 동시분석법의 검출한계 및 정량한계는 각각 ofloxacin 23.5 ppb, 35.3 ppb, norfloxacin 3.4 ppb, 5.1 ppb, ciprofloxacin 3.0 ppb, 4.5 ppb, enrofloxacin 2.5 ppb, 3.8 ppb수준이었다. 2. 인천 지역에서 도축한 닭고기 총 1,523수를 EEC-4-plate법으로 검사한 결과 양성반응을 보인 닭고기는 15수(육계 10, 토종닭 5)였으며, HPLC를 이용한 정밀검사결과 육계 5수에서 ciprofloxacin이 불검출 ∼0.04 ppm, enrofloxacin이 0.01∼0.69 ppm수준으로 검출되었으며, 토종닭 5수에서는 ciprofloxacin이 0.02∼0.12 ppm, enrofloxacin이 0.36∼6.79 ppm수준으로 검출되었다.

• 한국동물위생학회지
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• 제32권3호
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• pp.281-286
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• 2009

Fluoroquinolones in muscle and egg were separated by liquid extraction and determined. The analysis was carried out using following conditions; C18 column ($150{\times}4.6mm$, $5{\mu}m$), mobile phase composed of D.W. (containing 0.4% triethylamine and phosphoric acid) : methanol : acetonitrile (780:100:120, v/v/v), quarternary pump at a flow rate of 0.9ml/min and $20{\mu}l$ of injection volume, fluorescence detector with EX 278nm/Em 456nm. The calibration range of seven fluoroquinolones showed linearity ($r^2{\geq}0.999$) at concentration range of $0.025{\sim}0.8{\mu}g/ml$. The recoveries in fortified muscle and egg represented more than 81.3%. The detection limits for ofloxacin, norfloxacin, ciprofloxacin, enrofloxacin, danofloxacin, saraloxacin and orbifloxacin were 3.1, 2.5, 3.6, 1.7, 0.9, 2.5 and $2.1{\mu}g/kg$, respectively. We also monitored fluoroquinolones residue in the sample (chicken muscle 182, cattle muscle 140, pig muscle 139, egg 212) using EEC-plate (E. coli ATCC 11303) screening and HPLC confirmation methods. The screening test results, fluoroquinolones, antibacterial substances were all negative.