Korean Journal of Environmental Agriculture (한국환경농학회지)

The Korean Society of Environmental Agriculture (한국환경농학회)
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Development of Analytical Method for the Determination and Identification of Unregistered Pesticides in Domestic for Orange and Brown Rice(I) -Chlorthal-dimethyl, Clomeprop, Diflufenican, Hexachlorobenzene, Picolinafen, Propyzamide-

식품공전 분석법 미설정 농약의 잔류분석법 확립(I) -Chlorthal-dimethyl, Clomeprop, Diflufenican, Hexachlorobenzene, Picolinafen, Propyzamide-

  • Chang, Hee-Ra (Environmental Chemistry, HTRC, Hoseo Universitiy) ;
  • Kang, Hae-Rim (Environmental Chemistry, HTRC, Hoseo Universitiy) ;
  • Kim, Jong-Hwan (Environmental Toxicology Center, Korea Institute of Toxicology, KRICT) ;
  • Do, Jung-A (National Institute of Food and Drug Evaluation) ;
  • Oh, Jae-Ho (National Institute of Food and Drug Evaluation) ;
  • Kwon, Ki-Sung (National Institute of Food and Drug Evaluation) ;
  • Im, Moo-Hyeog (Korea Food and Drug Administration) ;
  • Kim, Kyun (Environmental Chemistry, HTRC, Hoseo Universitiy)
  • 장희라 (호서대학교 안전성평가센터) ;
  • 강혜림 (호서대학교 안전성평가센터) ;
  • 김종환 (안전성평가연구소 환경독성연구센터) ;
  • 도정아 (식품의약품안전평가원 화학물질과) ;
  • 오재호 (식품의약품안전평가원 화학물질과) ;
  • 권기성 (식품의약품안전평가원 화학물질과) ;
  • 임무혁 (식품의약품안전청 식품기준과) ;
  • 김균 (호서대학교 안전성평가센터)
  • Received : 2012.06.04
  • Accepted : 2012.06.25
  • Published : 2012.06.30
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Abstract

BACKGROUND: For the safety of imported agricultural products, the study was conducted to develop the analytical method of unregistered pesticides in domestic. The analytical method of 6 pesticides, chlorthal-dimethyl, clomeprop, diflufenican, hexachlorobenzene, picolinafen, and propyzamide, for a fast multi-residue analysis were established for two different type crops, orange and brown rice by GC-ECD and confirmed by mass spectrometry. METHODS AND RESULTS: The analytical method was evaluated to limit of quantification, linearity and recoveries. The crop samples were extracted with acetonitrile and performed cleanup by liquid-liquid partition and Florisil SPE to remove co-extracted matrix. The extracted samples were analyzed by GC-ECD with good sensitivity and selectivity of the method. The limits of quantification (LOQ) range of the method with S/N ratio of 10 was 0.02~0.05 mg/kg for orange and brown rice. The linearity for targeted pesticides were $R^2$ >0.999 at the levels ranged from 0.05 to 10.0 mg/kg. The average recoveries ranged from 74.4% to 110.3% with the percentage of coefficient variation in the range 0.2~8.8% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in brown rice. And the average recoveries ranged from 77.8% to 118.4% with the percentage of coefficient variation in the range 0.2~6.6% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in orange. Final determination was by gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM) to identify the targeted pesticides. CONCLUSION: As a result, this developed analytical method can be used as an official method for imported agricultural products.

수입 농식품에 대하여 국내에 등록되지 않아 식품공전 상의 분석법이 미확립된 chlorthal-dimethyl, clomeprop, diflufenican, hexachlorobenzene, picolinafen, propyzamide등 6종의 농약에 대해 GC-ECD로 다성분 동시분석법을 확립하였고, GC/MS로 확인하였다. 대상작물은 현미와 오렌지 2종을 선정하였고, 분석법은 식품의약품안전청에서 고시한 다종농약다성분 동시분석법을 적용하였다. 시료의 추출은 acetonitrile을 사용하였고 Florisil SPE 정제과정을 거쳤다. 분석법의 정량한계는 0.02~0.05 mg/kg 이었고, 직선성은 0.05~10.0 mg/kg 범위에서 $R^2$ >0.999였다. 평균회수율은 정량한계 수준에서 74.4~110.3%, 정량한계 수준의 10배에서 77.8~118.4%였으며, 변이계수는 전체시료에서 8.8% 이하로 잔류농약 분석기준인 회수율 70~120%와 10% 이내의 변이계수 조건을 충족시켰다. 이와 같이 확립된 6종의 다성분 분석법은 수입농산물 분석에 적용이 가능할 것으로 판단된다.

Keywords

References

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