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Multi-residue Pesticide Analysis in Cereal using Modified QuEChERS Samloe Preparation Method

곡물류 중 잔류농약 다성분 분석을 위한 개선된 QuEChERS 시료 정제법의 개발

  • Yang, In-Cheol (Enbio company) ;
  • Hong, Su-Myeong (Chemical Safety Division Department of Agro-food Safety, Rural Development Administration, National Academy of Agricultural Science) ;
  • Kwon, Hye-Young (Chemical Safety Division Department of Agro-food Safety, Rural Development Administration, National Academy of Agricultural Science) ;
  • Kim, Taek-Kyum (Chemical Safety Division Department of Agro-food Safety, Rural Development Administration, National Academy of Agricultural Science) ;
  • Kim, Doo-Ho (Chemical Safety Division Department of Agro-food Safety, Rural Development Administration, National Academy of Agricultural Science)
  • 양인철 ((주)인바이오 생명과학연구소) ;
  • 홍수명 (국립농업과학원 농산물안전성부 화학물질안전과) ;
  • 권혜영 (국립농업과학원 농산물안전성부 화학물질안전과) ;
  • 김택겸 (국립농업과학원 농산물안전성부 화학물질안전과) ;
  • 김두호 (국립농업과학원 농산물안전성부 화학물질안전과)
  • Received : 2013.08.21
  • Accepted : 2013.11.25
  • Published : 2013.12.31

Abstract

This study explored an efficient modified Quick, Easy, Cheap, Effective, Rugged and safe (QuEChERS) method combined with liquid chromatography-electrospray ionization with tandem mass spectrometric detection for the analysis of residues of 76 pesticides in brown rice, barley and corn including acidic sulfonylurea herbicides. Formic acid (1%) acid in acetonitrile and dispersive solid phase extractions used for extraction of pesticides and clean-up of the extract respectively. Two fortified spikes at 50 and 200 ng $g^{-1}$ levels were performed for recovery test. Mean recoveries of majority of pesticides at two spike levels ranged from 73.2 to 132.2, 80.9 to 136.8, 66.6 to 143.5 for brown rice, barley and corn respectively with standard error (CV) less than 10%. Good linearity of calibration curves were achieved with $R^2$ > 0.9907 within the observed concentration ranged. The modified method also provided satisfactory results for sulfonylurea herbicides. The method was applied to the determination of residues of target pesticides in real samples. A total of 26 pesticides in 36 out of 98 tasted samples were observed. The highest concentration was observed for tricyclazole at 1.17 mg $kg^{-1}$ in brown rice. This pesticide in two brown rice samples exceeded their MRLs regulated for rice in republic of Korea. Except tricyclazole none of the observed pesticides' concentration was higher than their MRLs. The results reveal that the method is effectively applicable to routine analysis of residues of target pesticides in brown rice, barley and corn.

Acknowledgement

Supported by : 국립농업과학원

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Cited by

  1. Gas Chromatographic Method for Multiresidue Analysis of Unregistered Pesticides in Imported Agricultural Commodities vol.19, pp.3, 2015, https://doi.org/10.7585/kjps.2015.19.3.161
  2. Development of Multi-residue Analysis of 320 Pesticides in Apple and Rice Using LC-MS/MS and GC-MS/MS vol.20, pp.2, 2016, https://doi.org/10.7585/kjps.2016.20.2.104