Inter-lab validation for the derivatization method by TFE/TFAA of acidic herbicides

산성 제초제류의 TFE/TFAA 유도체화 방법에 대한 실험실간 정도관리

  • Pyo, Hee-Soo (Bioanalysis & Biotransformation Research center, Korea Institute Science & Technology) ;
  • Park, Song-Ja (Bioanalysis & Biotransformation Research center, Korea Institute Science & Technology) ;
  • Lee, Kang-Jin (Water Analysis & Research Center, Woongjin coway CO. LTD) ;
  • Hong, Jong-Ki (Dept. of Pharmaceutical Science, Kyung Hee Univ.) ;
  • Shin, Ho-Sang (Dept. of Environmental Education, Kong Ju National Univ.)
  • 표희수 (한국과학기술연구원, 생체대사연구센터) ;
  • 박송자 (한국과학기술연구원, 생체대사연구센터) ;
  • 이강진 (웅진코웨이(주) 수질분석센터) ;
  • 홍종기 (경희대학교 약학과) ;
  • 신호상 (공주대학교 환경과학과)
  • Published : 2005.06.30

Abstract

A sensitive derivatization method by using the TFE/TFAA as derivative reagent is proposed for the determination of acidic herbicides in water, by using this method, method detection limits are improved by 10 times and sample volumes are decreased by 5 times compared with other methods such as U.S. EPA and SPEED 98. And also, in order to suggest higher creditable standard operating procedure (SOP), intra- and inter-lab validation test carried out by four laboratories include our lab. The results of intra and inter-lab validations in same experimental conditions show good linearity in given range of concentrations as a $0.1{\sim}10.0$ ng/ml, and range of accuracies and precisions show $-20.5{\sim}12.2$ bias%, $0.55{\sim}24.48%$ (for intra-lab validation) and $-6.66{\sim}0.80 bias%$, $1.92{\sim}13.86%$ (for inter-lab validation), respectively.

환경시료 중에 포함되어 있는 미량 산성농약을 분석하기 위하여 유도체화방법으로 TFE/TFAA를 사용하였으며, 물시료 분석에 있어 기존 U.S. EPA 혹은 일본의 SPEED 98 방법보다 시료양은 최대 1/5로 줄이고 검출한계는 최대 10배 이상 증가되는 결과를 얻을 수 있었다. 또한 보다 신뢰도 높은 표준분석법을 만들기 위해서 자체 정도관리 실험과 더불어 외부 연구기관에 의한 정도관리를 수행하였다. 정도관리 실험은 동일 조건에서 시료를 분석함으로써 검량선 작성 및 기지 농도에서의 정밀도와 정확도를 조사하였고, 그 결과 0.1 - 10 ppb 농도 범위에서 직선성 0.99 이상의 검량선을 얻을 수 있었으며, 각 실험실의 내부 정도관리 값은 정확도 $-20.5{\sim}12.2$ bias %와 정밀도는 0.55 - 24.48 %로 나타났으며, 실험실간 정확도는 -6.66 - 0.80 bias %와 정밀도는 1.92 - 13.86 %로 매우 우수한 결과를 나타내었다.

Keywords

References

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