The Analysis of Dioxin-like PCBs in Fishes and Shellfishes using Accelerated Solvent Extraction (ASE) System and Multilayer Column Chromatography

가속용매추출장치(ASE) 및 다층크로마토그래피를 이용한 어패류 중의 dioxin-like PCBs의 분석

  • Oh, Keum-Soon (Department of Food Safety Evaluation, Korea Food & Drug Administration) ;
  • Park, Seong-Soo (Seoul Regional of KFDA) ;
  • Chung, So-Young (Department of Food Safety Evaluation, Korea Food & Drug Administration) ;
  • Sho, You-Sub (Department of Food Safety Evaluation, Korea Food & Drug Administration) ;
  • Kim, Jung-Soo (Department of Food Safety Evaluation, Korea Food & Drug Administration) ;
  • Jang, Seoung-Chul (Department of Food Safety Evaluation, Korea Food & Drug Administration) ;
  • Lee, Jong-Ok (Department of Food Safety Evaluation, Korea Food & Drug Administration) ;
  • Kim, Hee-Yun (Gyeongin Regional of KFDA) ;
  • Woo, Gun-Jo (Department of Food Safety Evaluation, Korea Food & Drug Administration) ;
  • Suh, Jung-Hyuck (Department of Food Safety Evaluation, Korea Food & Drug Administration)
  • 오금순 (식품의약품안전청 식품평가부) ;
  • 박성수 (서울지방식품의약품안전청) ;
  • 정소영 (식품의약품안전청 식품평가부) ;
  • 소유섭 (식품의약품안전청 식품평가부) ;
  • 김정수 (식품의약품안전청 식품평가부) ;
  • 장승철 (식품의약품안전청 식품평가부) ;
  • 이종옥 (식품의약품안전청 식품평가부) ;
  • 김희연 (경인지방식품의약품안전청) ;
  • 우건조 (식품의약품안전청 식품평가부) ;
  • 서정혁 (식품의약품안전청 식품평가부)
  • Published : 2007.04.30

Abstract

In this study, an analytical method was optimized for detecting dioxin-like PCBs in fish and shellfish. Here, homogenized samples were extracted using an accelerated solvent extraction (ASE) system with 33 mL cell size. Multilayer column chromatography, which consisted of acidic, basic and neutral silica gels, was used for the clean up of the extracts. The instrumental analysis was executed by HRGC/HRMS to a resolution of 10,000 using 4 window multiple ion detection (MID) mode. For the results, the average recoveries ranged from 94.1 to 104.1% (${\pm}8.4$) and the limit of detection was approximately 0.1 pg/g at S/N ratio >3. Finally, the detected concentrations of dioxin-like PCBs for fish and shellfish were in the range of 0.030-1.836 pg TEQ/g.

식품 중에서 dioxin-like PCBs를 분석하기 위하여 가속용매추출기를 이용하여 추출하고 다층컬럼크로마토그래피를 이용하여 정제하는 분석법을 확립하였으며 어패류에 실제로 적용하여 그 오염수준을 조사하였다. 시료는 균질화하여 33 mL 추출 셀을 포함한 가속용매추출기를 이용하여 추출하였다. 추출액을 산성 실리카겔, 중성 실리카겔 및 염기성 실리카겔이 연속으로 충전된 컬럼을 통과하여 지방 및 방해성분을 제거하였다. 기기분석은 고분해능 질량분석기를 이용하여 분해능 10,000에서 4 window MID (multiple ion detection) mode로 분석하였다. 분석결과 평균 회수율은 94.1-104.1% (${\pm}8.4$)이었고 검출한계는 신호 대 잡은 비 (S/N)>3에서 0.1 pg/g이었다. 확립된 분석법을 이용하여 식품시료에 적용한 결과 dioxin-like PCBs의 오염수준은 0.030-1.836 pg TEQ/g이었다.

Keywords

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