Determination and confirmation of the carbendazim residue in soybean sprout

콩나물중 살균제 carbendazim 잔류분의 정량 및 확인

  • Kim, Young-Gook (Agriculture & Livestock Products Analysis Division, Health and Environment Institute of Chollanam-do) ;
  • Park, Jong-Tae (Agriculture & Livestock Products Analysis Division, Health and Environment Institute of Chollanam-do) ;
  • Hong, Suk-Soon (Agriculture & Livestock Products Analysis Division, Health and Environment Institute of Chollanam-do)
  • 김영국 (전라남도보건환경연구원 농축산물분석과) ;
  • 박종태 (전라남도보건환경연구원 농축산물분석과) ;
  • 홍석순 (전라남도보건환경연구원 농축산물분석과)
  • Published : 1998.12.30

Abstract

Tandem HPLC and atmospheric pressure chemical ionization(APcI) LC/MS method was used for the determination and confirmation of carbendazim residues in soybean sprout. Fluorescence(FL) detector was connected in tandem with the ultraviolet(UV) detector for dual detection of the carbendazim residue at the excitation and emission wavelength of 280 nm and 310 nm, respectively. The limit of detection for carbendazim was $0.1{\mu}g/kg$ sample. Recoveries of carbendazim from fortified soybean sprout at 0.5, 1.0 and 2.0 ppm were averaged 89.1%. Mass spectrometry using a APcI source confirmed the carbendazim residue in the soybean sprout sample. Fragmentation pattern on the APcI LC/MS spectrum of carbendazim was simpler than that from electron impact(EI) mass spectrum. Carbendazim produced 3 major ions including m/z 133, m/z 159 and m/z 191($M^{+}$). This method was sensitive enough to provide reliable and reproducible results for practical applications.

콩나물중 carbendazim 잔류분을 정량하고 확인할 수 있는 새로운 분석법을 확립하고자 tandem HPLC(UV & FL) 및 APcI를 source로 사용한 LC/MS를 이용하였다. 이를 위해 FL(fluorescence) 검출기를 UV(ultraviolet) 검출기와 나란히 연결하여 UV 검출기의 경우 280 nm 파장을 그리고 FL 검출기의 경우는 excitation파장과 emission파장을 각각 280 mn와 310 nm로 설정하였다. 분석결과 carbendazim의 검출한계는 $0.04{\mu}g/kg$이었다. 콩나물에 carbendazim을 0.5, 1.0 및 2.0 ppm 수준으로 첨가하여 회수율을 측정한 결과 그 평균값은 89.1%이었다. APcI source를 사용한 LC/MS 질량스펙트럼 방법은 콩나물중 carbendazim 잔류분을 최종 확인할 수 있었다. APcI LC/MS 방법은 전자충격에 의한 질량스펙트럼에 비해 훨씬 간단한 fragment를 형성할 뿐 만 아니라 carbendazim의 경우 m/z 133, m/z 159, m/z 191($M^{+}$)의 전형적인 fragment 이온을 형성하므로, 이 방법을 병행한다면 콩나물중 carbendazim 잔류분을 효과적으로 확인할 수 있을 것으로 사료되었다.