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2010년 국내산 및 수입 축산물의 잔류 동물용 의약품 탐색 조사
조병훈 ( Byung Hoon Cho ),박수정 ( Su Jeong Park ),김명애 ( Myeong Ae Kim ),신진영 ( Jin Young Shin ),김민경 ( Min Kyoung Kim ),강정우 ( Jeong Woo Kang ),임채미 ( Chae Mi Lim ),운재호 ( Jae Ho Woon ),손성완 ( Seong Wan Son ) 한국예방수의학회(구 한국수의공중보건학회) 2011 예방수의학회지 Vol.35 No.3
The Korean National Residue Program consists of three sampling plans for domestic and imported foods of animal origin: monitoring, surveillance/enforcement and exploratory testing. Monitoring and surveillance/enforcement testing programs are routinely implemented by 17 Provincial Veterinary Services for domestic products and two regional offices of Animal, Plant and Fisheries Quarantine and Inspection Agency (QIA) for imported products, respectively. The exploratory testing is designed to test substances which are not included in the list of monitoring and enforcement testing programs controlled by headquarter of QIA. In 2010, the exploratory testing was carried out in domestic and imported foods of animal origin for 24 veterinary drugs including florfenicol, clavulanic acid, four quinolones (nalidixic acid, difloxacin, marbofloxacin, orbifloxacin), two anthelmintics (closantel, levamisole), two sedatives (azaperone, carazolol), six glucocorticoids (dexamethasone, betamethasone, flumethasone, prednisone, prednisolone, methylprednisolone), eight non-steroidal anti-inflammatory drugs (phenylbutazone, paracetamol, carprofen, flunixin, ketoprofen, meloxicam, tolfenamic acid, acetylsalicylic acid). In the total of 1,153 domestic samples, only florfenicol was detected from 17 pig muscles at levels of 0.2~614 ng/g. Of 17 positive pig muscles, 16 samples were non-violative and one sample was violative. In the total of 1,065 imported samples, florfenicol was detected at 0.4 ng/g in one pork. Also, flunixin was detected at 22 ng/g in one beef.
김미경,조병훈,김동규,윤선종,임채미,박수정,김희진,김연희,김수연,윤소미,권진욱,손성완,정갑수,이주호,강문일,Kim, MeeKyung,cho, Byung-Hoon,Kim, Dong-Gyu,Yun, Seon Jong,Lim, Chae-Mi,Park, Su-Jeong,Kim, Heuijin,Kim, Yeon Hee,Kim, Soo-Yeon,Yun, So Mi,K 대한수의학회 2006 大韓獸醫學會誌 Vol.46 No.4
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.
유가공품 중 칼슘 및 프락토올리고당 영양강화 함량 분석
박지성,박재우,조병훈,송성옥,위성환,오순민,김진만,Park, Ji-Sung,Park, Jae-Woo,Cho, Byung-Hoon,Song, Sung-Ok,Wee, Sung-Hwan,Oh, Soon-Min,Kim, Jin-Man 한국축산식품학회 2013 한국축산식품학회지 Vol.33 No.6
본 연구는 시중에서 유통중인 유가공품 중 칼슘과 프락토올리고당 영양소 강조 또는 함유 표시 제품에 대해 실제 함량을 분석하였다. 칼슘 강화 유제품에 대하여는 우유류, 발효유류, 치즈류 등 40개 제품을 수집하여 칼슘 함량을 조사하였다. 그 결과 우유류 12제품의 1회 제공량당 칼슘 함량 표시는 105~500 mg (1.1~2.5 mg/mL)이었으며, 분석값은 1.0~2.4 mg/mL로 표시값에 대한 분석값은 87~127%이었다. 발효유류 12제품의 1회 제공량당 칼슘 함량 표시는 30~110 mg (0.4~1.4 mg/g)이었으며, 분석값은 0.3~1.6 mg/g로 표시값에 대한 분석값은 89~131%이었다. 치즈류 16제품의 1회 제공량당 칼슘 함량 표시는 84~2000 mg (3.5~20 mg/g)이었으며, 분석값은 4.2~23.0 mg/g으로 표시값에 대한 분석값은 83~127%이었다. 분석대상 시료의 칼슘함량 표시 대비 실제 분석값은 모두 80% 이상으로 축산물의 표시기준을 충족하였다. 프락토올리고당 강화 유제품에 대하여는 시중 유통 24개 제품에 대하여 그 함량을 조사한 결과 발효유 4.2~30.8 mg/g, 농후발효유 8.7~10.6 mg/g, 유음료 18.5 mg/mL, 연성가공치즈 1.3 mg/g으로 나타났다. 축산물의 표시기준에서 프락토올리고당에 대해서는 표시내용과 실제 함량 사이의 인정범위를 규정하고 있지는 않으나, 이들 24개 제품 중 실제 4개 제품에서는 명확한 함량이 표시되었으며, 분석값은 9.1~18.9 mg/g으로 표시량 대비 83~154%의 결과를 나타내었다. Nutrients fortified dairy products declare their contents on the label for nutrition claim and marketing. However, there are few monitoring studies about relations between actual quantities of fortified nutrients and the described ones on the label. This study was carried out for comparing actual fortified nutrient contents with labeled ones. Forty calcium fortified dairy products and twenty four fructooligosaccharides (FOS) fortified dairy products were sampled at supermarkets located in Anyang, Korea from March to November in 2010. Calcium contents were analyzed by using inductively coupled plasma optical emission spectrometry followed by microwave sample digestion, and FOS contents were analyzed by HPLC-ELSD followed by solvent extraction. In fresh milk, calcium contents ranged from 1.0 to 2.4 mg/mL, and those values were 87~127% of their labeled contents. In fermented milk products and cheeses, calcium contents ranged from 0.3 to 1.6 mg/g (89~131% of their labeled contents), 4.2 to 23.0 mg/g (83~127% of their labeled contents), respectively. FOS contents ranged from 9.09 to 18.89 mg/g in FOS contents labeled products and showed 83~154% compared to their labeled quantity, and ranged from 1.3~30.8 mg/g in products without quantity labeling. In conclusion, the amounts of calcium and FOS in dairy products were above 80% compared to their labeled ones and conformed to the Korean official livestock products labeling standard.
시료고체상분산(matrix solid phase dispersion)전처리법을 이용한 식육중 테트라사이클린계 항생물질 동시정량분석
강환구,손성완,조병훈,이혜숙,박신자,김재학,조명행,Kang, Hwan-goo,Son, Seong-wan,Cho, Byung-hoon,Lee, Hye-sook,Park, Shin-ja,Kim, Jae-hak,Cho, Myung-haing 대한수의학회 1996 大韓獸醫學會誌 Vol.36 No.3
Tetracycline antibiotics have been widely used not only therapeutics but feed additives. There are many methods for the isolation and determination of tetracycline antibiotics in animal muscle tissue. But those methods take much time and labor, so it is difficult to analyse many samples simultaneously. A rapid isolation method and liquid chromatographic determination of tetracycline antibiotics in animal muscle tissue (bovine, porcine, chicken) is presented. Blank control and tetracyclines fortified samples (0.5g) were blended with $C_{18}$ containing 0.05g each of oxalic acid and disodium ethylenediaminetetraacetate. After homogenize, homogenate was transferred to glass column made from 10ml glass syringe and compressed to 4~4.5ml volume. A column made from the $C_{18}$/meat matrix was washed with hexane (8ml) and dichloromethane (8ml, if needed), following which the tetracyclines were eluted,vith methanol or 0.01M methanolic oxalic acid (8ml). The eluates containing tetracyclines analytes were free from interfering compounds when analysed by HPLC with UV detection (photodiode array at 360nm). Standard curve for each tetracycline showed a linear response at the range of $0.05{\sim}1.0{\mu}g/ml$ and tetracycline antibiotics were eluted within 4ml of eluted volume. All tetracycline antibiotics except tetracycline were stable during the concentration process at $40^{\circ}C$ and time required for concentration was 3~4 hours. Fortified samples containing oxalic aicd and EDTA represented more good recoveries than those of not-contained sample. Recoveries were 91.8~110.1% (oxytetracycline; OTC), 57.7~79.5% (tetracycline; TC), 78.1~88.6% (chlortetracyclines; CTC) and 88.4~100.6% (doxycycline; DC) in pork tissue, 101.1~126.8% (OTC), 66.4~75.4% (TC), 79.2~88.1% (CTC) and 69.3~86.7% (DC) in beef tissue, and 90.8~95.6% (OTC), 66.2~84.4% (TC), 75.7~77.2% (CTC) and 55.6~80.7% (DC) in chicken muscle tissue. The detection limits validated in muscle tissue by this method were $0.05{\mu}g/g$ for OTC and TC, and $0.1{\mu}g/g$ for CTC and DC.