Korean Journal of Environmental Agriculture (한국환경농학회지)

The Korean Society of Environmental Agriculture (한국환경농학회)
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Application of Macroporous Diatomaceous Earth Column for Residue Analysis of Insecticide Endosulfan in Herbal Medicines

한약재 중 살충제 Endosulfan의 잔류분석을 위한 Macroporous Diatomaceous Earth 컬럼 적용

  • Hwang, Jeong-In (School of Applied Biosciences, Kyungpook National University) ;
  • Jeon, Young-Hwan (School of Applied Biosciences, Kyungpook National University) ;
  • Kim, Hyo-Young (School of Applied Biosciences, Kyungpook National University) ;
  • Kim, Ji-Hwan (School of Applied Biosciences, Kyungpook National University) ;
  • Lee, Yoon-Jeong (Division of Herbal Medicine Research, Korea Food and Drug Administration) ;
  • Park, Ju-Young (Division of Herbal Medicine Research, Korea Food and Drug Administration) ;
  • Kim, Do-Hoon (Division of Herbal Medicine Research, Korea Food and Drug Administration) ;
  • Kim, Jang-Eok (School of Applied Biosciences, Kyungpook National University)
  • 황정인 (경북대학교 응용생명과학부) ;
  • 전영환 (경북대학교 응용생명과학부) ;
  • 김효영 (경북대학교 응용생명과학부) ;
  • 김지환 (경북대학교 응용생명과학부) ;
  • 이윤정 (식품의약품안전청 생약연구과) ;
  • 박주영 (식품의약품안전청 생약연구과) ;
  • 김도훈 (식품의약품안전청 생약연구과) ;
  • 김장억 (경북대학교 응용생명과학부)
  • Received : 2011.03.02
  • Accepted : 2011.03.21
  • Published : 2011.03.31
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Abstract

BACKGROUND: Because dried herbal medicines have many active ingredients, it is not easy to determine the residue amount after extraction, partition and clean up of pesticides from them. Especially, liquid-liquid partition method is consuming many times and solvents. Macroporous diatomaceous earth(MDE) column was used to replace the separatory funnel for liquid-liquid extraction with dichloromethane to analyze the endosulfan and its metabolite. METHODS AND RESULTS: The residue analysis method using MDE column instead of liquid-liquid partition for determining insecticide endosulfan and its metabolite in 4 dried herbal medicines was developed by GC/MS. As a result, the recovery rates of the pesticides in 4 herbal medicines were ranged from 80.3 to 93.5% for ${\alpha}$-endosulfan, from 81.0 to 100.3% for ${\beta}$-endosulfan and from 80.6 to 95.6% for endosulfan sulfate, respectively. The coefficients of variation for triplicate were ranged from 1.1 to 3.4%. CONCLUSION: The improved methods are more ecofriendly, safer, faster and less laborious than conventional method by KFDA.

현재 식품의약품안전청에서 고시하고 있는 한약재 중 잔류 농약 분석법에 따라 강활, 박하, 천궁 및 황기 시료 중 endosulfan과 그 분해산물인 endosulfan sulfate를 분석한 결과 많은 간섭물질의 등장과 낮은 회수율 등의 문제점을 확인하였다. 이에 고시된 시험법의 액-액 분배 과정을 대신하여 MDE column을 적용하여 ${\alpha}$-endosulfan 80.3 ~ 93.5%, ${\beta}$-endosulfan 81.0 ~ 100.3%, endosulfan sulfate 80.6 ~ 95.6%의 회수율과 1.1 ~ 3.4%의 변이계수(CV)를 얻었으며 이러한 결과는 잔류농약 분석기준을 만족하였다. MDE column의 사용으로 액-액 분배 과정을 대신하면서 발암가능 물질인 dichloromethane 사용을 배제할 수 있어 분석자의 안전성 향상, 노동력 및 전처리 시간의 절감, 발생되는 폐액 감소, 액-액 분배시 emulsion 현상의 해소, 분석자간의 재현성 양호 등의 이점도 얻을 수 있었다.

Keywords

References

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