GC/MS를 이용한 뇨중 몇가지 농약의 분석

Analysis of some pesticides in urine by GC/MS

  • 박성수 (식품의약품안전청 생약제제과) ;
  • 박송자 (한국과학기술연구원 생체대사연구센타) ;
  • 표희수 (한국과학기술연구원 생체대사연구센타) ;
  • 조정희 (식품의약품안전청 생약제제과) ;
  • 김혜수 (식품의약품안전청 생약제제과) ;
  • 박택규 (건국대학교 이과대학 화학과)
  • Park, Seong-Soo (Division of Natural Medicinal Products, Korea Food and Drug Administration) ;
  • Park, Song-Ja (Bioanalysis and Biotransformation Research Center, Korea Institute of Science and Technology) ;
  • Pyo, Hee-Soo (Bioanalysis and Biotransformation Research Center, Korea Institute of Science and Technology) ;
  • Cho, Jung-Hee (Division of Natural Medicinal Products, Korea Food and Drug Administration) ;
  • Kim, Hye-Soo (Division of Natural Medicinal Products, Korea Food and Drug Administration) ;
  • Park, Taek-Kyu (Dept. of Chemistry, Konkuk University)
  • 발행 : 2000.03.31

초록

이 연구는 뇨시료 중에서 검출될 수 있는 9종의 농약에 대하여 HP-1 capillary column(25 m ${\times}$ 0.2 mm I.D., $0.33{\mu}m$ film thickness)을 사용하여 GC/MS/SIM방법으로 동시에 분리 정량할 수 있는 분석방법을 확립하였다. 9종의 농약에 대한 뇨시료로 부터의 추출은 pH 7.0에서 diethyl ether를 사용한 LLE 방법으로 대체로 높은 회수율과 10%이하의 상대표준편차를 나타내었다. SIM 방법으로 얻은 농약의 표준검정곡선은 농도범위 $4.0{\sim}1,000$ ppb에서 직선성이 양호하였고 정량한계는 $0.4{\sim}2.0$ ppb를 나타내었다. 실제로 농약을 살포한 다음 24시간 동안 배설된 뇨시료 중에서 각 농약 물질에 대한 parent form은 모두 검출되지 않았으며, phenthoate를 포함하는 농약을 살포한 후 채취된 뇨시료에서 대사체로 예상되는 ${\alpha}$-hydroxybenzeneacetic acid를 확인하였다.

The purpose of this study is to establish the assessment techniques of hazardous chemicals by the development of analytical method of biological samples. In this study, we have developed an extraction method of nine pesticides used for rice paddy that resulted in high recovery from the spiked human urine by the liquid-liquid extraction with diethyl ether at pH 7.0. Calibration curve obtained from each pesticide standard using by gas chromatography/mass spectrometry/selected ion monitoring has shown good linearity and detection limits were the range of $0.4{\sim}2.0$ ng/mL in urine. As a biological monitoring, urine samples of local farmers exposed directly to nine pesticides in the field were collected and analyzed by GC/MS. Of the tested pesticides, metabolites of phenthoate assumed were identified by GC/MS analysis. No parent compound was detected.

키워드