한국식품위생안전성학회지 (Journal of Food Hygiene and Safety)

  • 제29권4호
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  • Pages.292-298
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  • 2014
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  • 1229-1153(pISSN)
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  • 2465-9223(eISSN)
한국식품위생안전성학회 (The Korean Society of Food Hygiene and Safety)
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Development and Validation of an Analytical Method for Tridemorph Determination in Tea Samples by Liquid Chromatograph-Electrospray Ionization-Tandem Mass Spectrometry

  • Do, Jung-Ah (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation) ;
  • Park, Hyejin (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation) ;
  • Kwon, Ji-Eun (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation) ;
  • Cho, Yoon-Jae (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation) ;
  • Chang, Moon-Ik (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation) ;
  • Oh, Jae-Ho (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation) ;
  • Hwang, In-Gyun (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation)
  • 투고 : 2014.05.19
  • 심사 : 2014.09.24
  • 발행 : 2014.12.31
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초록

차 중에 있는 살균제 tridemorph의 잔류량을 검사하기 위해 LC-ESI-MS/MS를 이용한 정확하고 감도가 좋은 분석방법을 개발하였다. Tridemorph 잔류물은 샘플을 수화한 후 acetonitrile로 추출하고, NaCl을 이용한 액-액 분배, $NH_2$ 카트리지 정제를 거쳐 기기분석을 수행하였다. 직선성은 $0.02{\sim}1.0{\mu}gmL^{-1}$ 범위에서 상관계수($r^2$) 0.9999로 높은 직선성을 보였다. 0.02와 $0.05mgkg^{-1}$ 처리수준으로 회수율을 실험한 결과는 75.0~84.7% 이었으며, 상대표준편차는 10% 미만이었다. 분석방법의 검출한계와 정량한계는 각각 0.01와 $0.02mgL^{-1}$ 이었다. 이러한 결과들을 통해 확립된 분석법은 차 중 tridemorph의 잔류량 분석에 적합함을 확인할 수 있었다.

Tridemorph is a systemic morpholine fungicide for crops. The objective of this study was to develop reliable and sensitive analytical method for determination of tridemorph residues in tea samples for ensuring the food safety. Tridemorph residues in samples were extracted with acetonitrile after hydration, partitioned with saline water, and then purified using an aminopropyl ($NH_2$) SPE cartridge. The purified samples were detected and quantified using LC-ESI-MS/MS. The linear detection limits for tridemorph ranged from 0.02 to $1.0mgL^{-1}$ with a correlation coefficient of 0.9999. The method was validated using tea samples spiked with tridemorph at different concentration levels (0.02 and $0.05{\mu}gmL^{-1}$). The average recovery ranged between 75.0 and 84.7% with relative standard deviations less than 10%. The LOD and LOQ were 0.01 and $0.02mgL^{-1}$, respectively. The developed method was applied successfully to the identification of tridemorph in real tea samples obtained from different sources, and tridemorph was not detected in any of the samples. The results show that the developed analytical method is accurate and suitable for tridemorph determination in tea samples.

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