Analytical Science and Technology (분석과학)

The Korean Society of Analytical Sciences (한국분석과학회)
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Determination of tetracycline antibiotics in food

식품 중 테트라싸이클린계 항생물질의 분석

  • Park, Dongmi (Residue & Chemicals Division, Korea Food & Drug Administration) ;
  • Jeong, Jiyoon (Residue & Chemicals Division, Korea Food & Drug Administration) ;
  • Chang, Moonik (Residue & Chemicals Division, Korea Food & Drug Administration) ;
  • Im, Moohyeog (Residue & Chemicals Division, Korea Food & Drug Administration) ;
  • Park, Kunsang (Residue & Chemicals Division, Korea Food & Drug Administration) ;
  • Hong, Mooki (Residue & Chemicals Division, Korea Food & Drug Administration)
  • 최동미 (식품의약품안전청, 잔류화학물질과) ;
  • 정지윤 (식품의약품안전청, 잔류화학물질과) ;
  • 장문익 (식품의약품안전청, 잔류화학물질과) ;
  • 임무혁 (식품의약품안전청, 잔류화학물질과) ;
  • 박건상 (식품의약품안전청, 잔류화학물질과) ;
  • 홍무기 (식품의약품안전청, 잔류화학물질과)
  • Received : 2005.04.08
  • Accepted : 2005.04.21
  • Published : 2005.06.25
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Abstract

A selective method of high performance liquid chromatography with UV detector has been applied to determine 4 tetracycline antibiotics in the animal food, simultaneously. The targets were chlortetracycline (CTC), doxycycline (DC), oxytetracycline (OTC), and tetracycline (TC) that are used routinely in veterinary medicine for prevention and control of disease. Food samples were beef, pork, chicken, milk, whole egg, flatfish (Limanda yokohamae), jacopever (Sebastes hubbsi), seabream (Chrysophrys major), eel (Anguilla japonica) and lobster (Hommarus americanus). After extracting food samples with 20% trichloroacetic acid and McIlvaine buffer, they were purified by a $C_18$ SPE cartridge with 0.01M methanolic oxalic acid solution. The concentrated residue was re-dissolved in methanol, filtered, cleaned up and analyzed on a $C_18$ column. The mobile phase was a mixture of 0.01M oxalic acid and acetonitrile with a gradient ratio from 85:15 to 60:40. The UV wavelength was 365 nm. The overall recoveries were ranged from 71% to 98% and the limit of detections were 0.022 for CTC, 0.012 for DC and OTC and 0.009 mg/kg for TC at signal/noise > 3, respectively. As results, CTC, DC and TC were not detected in all selected food samples, however, OTC was detected in meat and fishes. The determined level of OTC was 0.04 ppm for pork, 0.17 ppm for flatfish and 0.05 and 0.08 ppm for jacopever, that were within the Maximum Residue Limits (MRLs) in the food.

고속액체크로마토그라피를 이용하여 동물성 식품 중 테트라싸이클린계 항생물질의 동시분석을 시도하였다. 대상물질은 동물의 질병치료.예방, 성장촉진 및 사료효율 개선에 널리 사용되는 클로르테트라싸이클린, 독시싸이클린, 옥시테트라싸이클린 및 테트라싸이클린이었으며, 대상식품은 쇠고기, 돼지고기, 닭고기, 우유, 계란, 넙치, 우럭, 참돔, 뱀장어 및 바다가재이었다. 시료를 McIlvaine 완충액 및 20% 삼염화초산으로 추출한 후 $C_18$ 카트리지로 정제하여 고속액체크로마토그라피로 분석하였다. 이동상으로는 0.01M 수산과 아세토니트릴의 혼합용액을 85:15에서 60:40까지 기울기로 사용하였으며 UV의 검출파장은 365 nm 이었다. 평균 회수율은 71-98% 이었으며, 검출한계는 신호대 잡음비 3 이상에서 클로르테트라싸이클린은 0.022, 독시싸이클린은 0.012, 옥시테트라싸이클린은 0.012 및 테트라싸이클린은 0.009 mg/kg이었다. 대부분의 시료에서 클로르테트라싸이클린, 독시싸이클린 및 테트라싸이클린은 검출되지 않았으나, 돼지고기, 넙치 및 참돔(2시료)에서 옥시테트라싸이클린이 각각 0.04, 0.17, 0.05 및 0.08 mg/kg로 모두 잔류허용기준을 초과하지 않은 수준으로 검출되었다.

Keywords

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