Journal of Food Hygiene and Safety (한국식품위생안전성학회지)

The Korean Society of Food Hygiene and Safety (한국식품위생안전성학회)
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Development of LC-MS/MS Quantitation Method for Ethoxyquin in Fishery Products

수산물 중 에톡시퀸의 LC-MS/MS 정량분석법 개발

  • Shin, Dasom (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Chae, Young-Sik (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Kang, Hui-Seung (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Lee, Soo-Bin (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Cho, Yoon-Jae (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Cheon, So-Young (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Jeong, Jiyoon (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Rhee, Gyu-Seek (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation)
  • 신다솜 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 채영식 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 강희승 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이수빈 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 조윤제 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 천소영 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 정지윤 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이규식 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과)
  • Received : 2016.09.13
  • Accepted : 2016.09.30
  • Published : 2016.12.30
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Abstract

Ethoxyquin (EQ, 1,2-dihydro-6-ethoxy-2,2,4-trimethyl-quinoline) is quinoline-based antioxidant used in the animal feed and food industry to protect the raw materials and final products against oxidation. In recent years the use of synthetic antioxidants in fishmeal ingredients carry-over to farmed fish fillets has received increasing attention in food safety. This study was conducted to develop an analytical method to determine EQ in aquatic products. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with 1 N HCl (in case of flatfish extracted with 1 N HCl containing 10% acetonitrile). Then, solid phase extraction (SPE) was used for the cleanup. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.99, analyzed at 0.005-0.2 mg/kg concentration. The developed method was validated according to the Codex Alimentarius Commission (CAC) guideline. The limits of quantitation for EQ were 0.01 mg/kg. Average recoveries ranged from 81.3% to 107%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was below 10%. The analytical method was characterized with high accuracy and acceptable sensitivity to meet CODEX guideline requirements and would be applicable to analyze the EQ residue in aquatic products.

본 연구는 수산물 중 에톡시퀸 정량시험법을 확립하여 국내 생산 및 수입 양식 수산물에 대한 잔류할 수 있는 동물용의약품인 에톡시퀸에 대한 안전관리 강화기반을 위해 마련되었다. LC-MS/MS를 이용하여 신속하고 효과적으로 정량성 및 정밀성을 확보하였으며, 확립된 시험법의 선택성, 정량한계 및 회수율에 대한 검증을 통하여 에톡시퀸 시험법으로서의 유효성을 확인하였다. 표준용액을 정량한계를 포함한 농도에 따라 검량선을 작성한 결과 $r^2$> 0.99 이상의 직선성을 확인하였으며, 산성용매로 추출 후 MCX 카트리지를 이용해 정제하였다. 본 실험에서의 검출한계는 0.001 mg/kg, 정량한계는 0.01 mg/kg 수준이었고, 평균 회수율은 81.3~107%이었다. 또한, 분석오차는 10% 이하로 정확성 및 재현성이 우수하였으며, CODEX 가이드라인 규정에 만족하는 수준이었다. 따라서, 개발된 시험법은 안전한 국내유통 수산물과 국민보건을 위해 지속적인 잔류실태조사에 활용되고, 수산물 중 잔류동물용의약품의 안전관리에 기여할 것으로 판단된다.

Keywords

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