Korean Journal of Veterinary Service (한국동물위생학회지)

The Korean Society of Veterinary Service (한국동물위생학회)
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Determination and survey of tetracyclines residue in honey by high performance liquid chromatography

액체크로마토그래피를 이용한 벌꿀 중 테트라싸이클린계 항생물질의 정량분석 및 잔류조사

  • Lee Sung-Mo (Incheon Metropolitan City Institute of Health & Environment) ;
  • Park Eun-Jeong (Incheon Metropolitan City Institute of Health & Environment) ;
  • Hong Jee-Young (Incheon Metropolitan City Institute of Health & Environment) ;
  • Kim Jung-Im (Incheon Metropolitan City Institute of Health & Environment) ;
  • Lee Jung-Goo (Incheon Metropolitan City Institute of Health & Environment) ;
  • Hwang Hyun-Soon (Incheon Metropolitan City Institute of Health & Environment) ;
  • Kim Yong-Hee (Incheon Metropolitan City Institute of Health & Environment)
  • 이성모 (인천광역시 보건환경연구원) ;
  • 박은정 (인천광역시 보건환경연구원) ;
  • 홍지영 (인천광역시 보건환경연구원) ;
  • 김정임 (인천광역시 보건환경연구원) ;
  • 이정구 (인천광역시 보건환경연구원) ;
  • 황현순 (인천광역시 보건환경연구원) ;
  • 김용희 (인천광역시 보건환경연구원)
  • Published : 2005.09.01
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Abstract

Oxytetracycline, tetracycline, chlortetracycline and doxycycline in honey were separated by solid phase extraction (SPE) and determined with high performance liquid chromatography (HPLC) with UV/Visible detector. Analysis was carried out using following conditions: XTerra $C_8$ column $(3.9\times150mm\;i.d. 5{\mu}m)$, mobile phase composed of 0.01M oxalic acid : methanol : acetonitrile (820 : 80 : 100, v/v/v), isocratic pump at a flow rate of 0.9 ml/min. and $50{\mu}l$ of injection volume, UV/Visible detector with wavelength of 360nm. The calibration curves of four tetracyclines showed linearity $(\gamma^2>0.999)$ at concentration range of $100\~1,000 ng/ml$. The recoveries in fortified honey represented more than $70\%$ with low coefficient of variation $(<10\%)$ for concentration range of four tetracyclines. The detection limits for oxytetracycline, tetracycline, chlortetracycline and doxycycline were 13.8, 14.6, 26.2 and 24.9ng/g in acacia honey. respectively. We also monitored tetracyclines residue in domestic honey [n : 38, acacia (20), wild flower (18) ] and foreign honey [n=22, legally distributed (13), illegally distributed (9)] using modified Charm II screening and HPLC confirmation methods. Seven of the 60 samples $(11.7\%)$ were suspect positive using modified Charm II screening test. Chlortetracycline residue was found in one foreign honey (illegally distributed) tested at concentrations of 0.22 ppm. Conclusively, for more effective control of tetracyclines used in beekeeping should be further survey for residues in honey and also national guidelines (maximum residue limit : MRL) and methods should be obligatory.

Keywords

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