• Journal of Applied Biological Chemistry
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• 제64권2호
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• pp.177-184
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• 2021

축산용 항생제는 투여된 양의 일부만이 체내에서 사용되며 나머지는 분뇨로 배출되며 이를 활용한 퇴비를 농경지에 살포함으로써 농업환경에 유입되어 2차 오염 등을 초래하고 있다. 따라서, 농업환경 중 항생제 관리기준 설정 등 사후 관리 기술이 필요하다. 본 연구는 국내 사용빈도가 높은 것으로 알려진 tetracycline 및 sulfonamide 계열 등의 항생제를 대상으로 매체별 잔류량을 비교하고 퇴비 시용 전·후 농경지 토양 중 잔류항생제의 위해성을 평가하기 위하여 수행되었다. Buffer 및 SPE를 사용한 전처리 방법은 ppb 수준에서 70% 이상의 회수율을 나타냈으며, 검출한계(LOD)의 범위는 퇴비와 토양에서 각각 0.13-0.46 ㎍/kg과 0.05-0.25 ㎍/kg이었다. 잔류 항생제 분석결과 퇴비 중 tetracycline 계열 항생제의 잔류 농도는 5.38-196.0 ㎍/kg, sulfonamide 계열은 below the detection of limit (BDL)-259.0 ㎍/kg 수준으로 검출되었다. 농경지 토양의 경우 각각 0.30-53.3 ㎍/kg, BDL-4.16 ㎍/kg의 잔류 수준을 나타냈으며 토양분배계수(Kd) 값이 높은 tetracycline 계열 항생제의 잔류 농도가 sulfonamide 계열보다 높았다. 퇴비 시용 전후의 농경지 토양의 항생제에 대한 인체위해도는 항생제 종류에 따른 차이가 있었으나, 전체 HQ가 1 이하에서 안전하다는 기준에 의하면 조사된 항생제 5종 모두 인체 위해성이 매우 낮았으며 시용 전·후의 영향이 전체 위해도에 미치는 비율을 고려하면, 퇴비시용이 토양의 항생제에 대한 인체위해성에 미치는 영향은 미비한 것으로 판단되었다.

• 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.

• 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 $100\;{\mu}g/kg$.

• 한국동물위생학회지
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• 제20권1호
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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).

• 분석과학
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• 제20권1호
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• pp.84-90
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• 2007

식품중 설폰아마이드계 동물용의약품 11종을 분석하기 위하여 고속액체크로마토그라피를 이용하여 동시분석을 시도하였다. 대상물질은 설파클로로피리다진(SCP), 설파디아진(SDZ), 설파디메톡신(SDM), 설피속사졸(SSX), 설파메라진(SMZ), 설파메타진(SMT), 설파메톡사졸(SMX), 설파메톡시피리다진(SMP), 설파모노메톡신(SMM), 설파퀴녹살린(SQX) 및 설파치아졸(STZ)이었다. 대상식품은 축산식품인 소고기, 돼지고기, 닭고기, 우유 및 계란 5품목이었으며, 전국 6대도시인 서울, 부산, 대전, 인천, 목포, 강릉에서 수집하였다. 시료에 인산나트륨 및 아세토니트릴을 가하여 균질화한 후 핵산을 가하여 추출하고 고속액체크로마토그라피로 분석하였다. 이동상으로는 5 mM 제1인산칼륨용액(pH 3.25)과 메탄올의 혼합용액을 100:0에서 30:70까지 그래디언트로 사용하였으며 UV의 검출파장은 270 nm이었다. 평균 회수율은 75~95%이었으며, 검출한계는 신호대 잡음비 3 이상에서 대상물질에 따라 최저 SMT 0.004에서 최고 STZ 0.007 mg/kg로 나타났다. 대부분의 시료에서 설폰아미이드계 동물용의약품은 검출되지 않았으나, 소고기(2시료)에서 설파모노메톡신이 각각 0.03, 0.06 mg/kg 수준으로 검출되었으며 잔류허용기준 이하로 평가되었다.

• 대한수의학회지
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• 제46권4호
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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.