DOI QR코드

DOI QR Code

MSPD와 HPLC를 이용한 돼지고기 및 광어 중의 테트라싸이클린계 항생제와 sulfonamide의 다성분 잔류분석법 개발

Simultaneous Determination of Tetracyclines and Sulfonamides Residues in Pork and Flatfish Using Matrix Solid Phase Dispersion (MSPD) Extraction and HPLC

  • 길근환 (농촌진흥청 국립농업과학원) ;
  • 고광용 (충남대학교 농화학과) ;
  • 이용재 (KT&G 중앙연구원) ;
  • 박혜진 (사우스다코타 주립대학교 식품화학부) ;
  • 이규승 (충남대학교 농화학과)
  • Gil, Geun-Hwan (National Academy of Agricultural Science, RDA) ;
  • Ko, Kwang-Yong (Dept. of Agriculture Chemistry, Chungnam National University) ;
  • Lee, Yong-Jae (Central Research Institute, KT&G) ;
  • Park, Hye-Jin (Food Science Department South Dakota State University) ;
  • Lee, Kyu-Seung (Dept. of Agriculture Chemistry, Chungnam National University)
  • 발행 : 2009.09.30

초록

HPLC를 이용한 분석은 항균, 항생제의 정량분석에 있어 가장 널리 이용되고 있으며, 최근에 개발된 MSPD방법은 고정상을 직접 갈아서 추출, 정제하는 방법으로 전처리 시 그조작이 간단하며, 유기용매가 적게 들고 전처리 시간이 짧다는 장점이 있다. 본 연구는 HPLC와 MSPD방법을 이용하여 가축 중 소비량이 가장 많은 돼지고기와 생선 중 회로 가장 많이 소비되는 광어에 대하여, 식품 중 잔류 가능성이 높은 tetracycline계 항생제 3종(oxytetracycline, tetracycline, chlortetracycline)과 sulfonamide(sulfadimethoxine, sulfamerazine, sulfamethazine, slfaquinoxaline, sulfamonomethoxine) 5종의 동시분석방법을 개발코자 하였다. HPLC의 최적 분석조건으로 파장은 tetracycline계 항생물질은 360 nm에서 sulfonamide는 270 nm였으며, 이동상은 TC와 SMR이 분리되는 시점인 15분까지는 pH 4.5, oxalic acid : acetonitrile (78.5 : 21.5, v/v)로 분석하고 이후 30분까지는 pH 6.1, oxalic acid : acetonitrile (78.5 : 21.5, v/v)로 분석을 실시하였을 때 기존의 실험방법보다 피크의 분리도와 검출한계의 개선이 이루어졌으며 이를 토대로 8가지 성분의 MRLs인 $0.1{\sim}0.2mg{\cdot}kg^{-1}$까지 충분히 분석이 가능하였다. MSPD 적용을 위한 시료의 전처리 방법개선은 기존의 0.5 g으로 제한된 시료량을 3 g으로 늘릴 수 있었고 dichloromethane 20 mL와 methanol 20 mL로 연속적으로 8가지 성분을 동시에 용출시켜 sulfonamide는 $80.25{\sim}101.25%$, tetracycline계 항생물질은 $85.77{\sim}121.42%$의 회수율을 얻을 수 있었다.

키워드

tetracyclines;sulfonamides;pig muscle;flatfish;MSPD;HPLC

참고문헌

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피인용 문헌

  1. Simultaneous Determination of Penicillin Antibiotics in Meat using Liquid Chromatography Tandem Mass Spectrometry vol.29, pp.2, 2014, https://doi.org/10.13103/JFHS.2014.29.2.131