Studies on the Simultaneous Analysis of Organochlorine Pesticide Residues by Gas-Liquid Chromatography (I). Solvent Extraction and Cleanup of Pesticides

기체-액체 크로마토그래피에 의한 잔류 유기염소제 농약들의 동시 분석에 관한 연구 (제1보). 농약의 용매추출 및 불순물 제거

  • Taek-Jae Kim (Chemical Analysis Lab., Korea Advanced Institute of Science and Technology) ;
  • Song-Ja Park (Chemical Analysis Lab., Korea Advanced Institute of Science and Technology) ;
  • Young-Sang Kim (Department of Chemistry, Korea University)
  • 김택제 (한국과학기술원 화학분석실) ;
  • 박송자 (한국과학기술원 화학분석실) ;
  • 김영상 (고려대학교 문리대학 화학과)
  • Published : 1985.10.20

Abstract

The solvent extraction and cleanup processes for the simultaneous gas-liquid cliromatographic determination of 16 kinds of organochlorine pesticide residues were investigated. The pesticides were extracted out from-various crops with the aqueous acetone solution acidified (pH < 1.5) by adding conc. $H_3PO_4$. Most of the pesticides were partitioned from the solution with petroleum ether. Evaporated the extracting solvent, the residues were dissolved in ethylether-petroleum ether (6 : 94) eluent and eluted through the Florisil column activated at 650$^{\circ}$C for 2.5hrs. The extraction efficiency was over 94% and impurities were effectively removed by the column chromatography.

농산물에 잔류되어 있는 16종의 유기염소제 농약들을 기체-액체 크로마토그래피(GLC)로 동시에 정량하기 위하여 필요한 전처리 과정인 용매추출과 불순물 제거(Cleanup) 처리에 대하여 조사 검토 하였다. 농산물로 부터 농약들을 $H_3PO_4$와 물을 가한 강산성(pH 1.5이하)의 actone용액으로 녹여낸 다음, petroleum ether를 분배 용매로 사용하여 농약을 추출시켰다. 추출물에서 용매를 증발시켜 날려보내고 ethylether-petroleum ether (6 : 94) 용리액으로 녹여서 650$^{\circ}$C에서 활성화 시킨 Florisil관을 통과시켜 불순물을 제거 하였다. Petroleum ether에 의한 추출효과는 94%이상으로 AOAC법 보다는 우수 하였고, Florisil관 크로마토그래피법에 의해 불순물이 제거되었다.

Keywords

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