Analytical Science and Technology (분석과학)

The Korean Society of Analytical Sciences (한국분석과학회)
권호 표지

Determination of Polybrominated Diphenyl Ethers(PBDEs) in Soil using Gas Chromatography/Isotope Dilution Mass Spectrometry

기체크로마토그래피/동위원소 희석 질량분석법을 이용한 토양 중 폴리브롬화 디페닐에테르의 분석법

  • Na, Yuncheol (Hazardous Substance Research Team, Korea Basic Science Institute) ;
  • Chang, Yoon-Seok (School of Environmental Science and Engineering, Pohang University of Science and Technology) ;
  • Kim, Hai-Dong (Department of Chemistry, KyungHee University) ;
  • Hong, Jongki (Hazardous Substance Research Team, Korea Basic Science Institute)
  • 나윤철 (한국기초과학지원연구원, 유해물질분석연구팀) ;
  • 장윤석 (포항공과대학교 환경공학부) ;
  • 김해동 (경희대학과 화학과) ;
  • 홍종기 (한국기초과학지원연구원, 유해물질분석연구팀)
  • Received : 2003.10.28
  • Accepted : 2003.12.15
  • Published : 2004.02.25
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Abstract

An analytical method of polybrominated diphenyl ethers in soil samples by isotope dilution method using gas chromatography/mass spectrometry (GC/MS)-selected ion monitoring (SIM) was described. PBDEs in soil were extracted with soxhlet extractor and then silica and florisil solid phase extraction (SPE) methods as purification of extract were compared. After clean-up, the extractions were analyzed by GC/MS with SIM mode. Quantitation was performed isotope dilution method using four $^{13}C$ isotopically labeled PBDEs as internal standards. This developed method was validated for eight congeners of PBDEs in the concentration range 0.04~4 ng/g in soil and the average recovery of the analytes ranged 30.8~110.8% for florisil and 44.4~110.7% for silica, respectively. The method detection limits of PBDEs were 0.04~0.3 ng/g.

본 연구에서는 토양중에 존재하는 폴리브롬화 디페닐에테르 (polybrominated diphenyl ethers, PBDEs)를 동위원소희석법을 이용한 기체크로마토그래피/질량분석기-선택이온검색법에 의해 검출하는 분석방법을 소개하였다. 토양 중 PBDEs는 속실렛 장치로 추출하고 실리카와 플로리실 흡착제를 이용한 고체상 추출법을 비교하였다. 정제 후 추출물은 기체크로마토그래피/질량분석기-선택이온검색방법으로 분석하였으며, 동위원소로 치환된 4종의 PBDEs를 내부표준물질로 이용한 동위원소 희석법으로 8종의 PBDEs를 정량하였다. 속실렛추출 후 플로리실과 실리카 카트리지를 통한 회수율은 각각 30.8~110.8%, 44.4~110.7%이었다. 이 분석법의 검출한계는 0.04~0.3 ng/g로 나타났다.

Keywords

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