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

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.

Keywords

chlortetracycline;doxycycline;oxytetracycline;tetracycline;food;HPLC

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