Determination of mandipropamid residues in agricultural commodities using high-performance liquid chromatography with mass spectrometry

고성능액체크로마토그래피를 이용한 농산물 중 Mandipropamid의 잔류분석법 확립

  • Kwon, Chan Hyeok (Food Safety Evaluation Department, KFDA) ;
  • Chang, Moon Ik (Food Safety Evaluation Department, KFDA) ;
  • Im, Moo Hyeog (Food Safety Evaluation Department, KFDA) ;
  • Choi, Hoon (Food Safety Evaluation Department, KFDA) ;
  • Jung, Da I (Food Safety Evaluation Department, KFDA) ;
  • Lee, Su Chan (Food Safety Evaluation Department, KFDA) ;
  • Yu, Jin Young (Food Safety Evaluation Department) ;
  • Lee, Young Deuk (Division of Life and Environmental Science, Daegu University) ;
  • Lee, Jong Ok (Food Safety Evaluation Department, KFDA) ;
  • Hong, Moo Ki (Food Safety Evaluation Department, KFDA)
  • 권찬혁 (식품의약품안전청 식품평가부) ;
  • 장문익 (식품의약품안전청 식품평가부) ;
  • 임무혁 (식품의약품안전청 식품평가부) ;
  • 최훈 (식품의약품안전청 식품평가부) ;
  • 정다이 (식품의약품안전청 식품평가부) ;
  • 이수찬 (식품의약품안전청 식품평가부) ;
  • 유진영 (식품의약품안전청 식품평가부) ;
  • 이영득 (대구대학교 생명환경학부) ;
  • 이종옥 (식품의약품안전청 식품평가부) ;
  • 홍무기 (식품의약품안전청 식품평가부)
  • Received : 2008.08.01
  • Accepted : 2008.10.16
  • Published : 2008.12.25

Abstract

Mandipropamid is a new mandelamide-type fungicide to control foliar Oomycete pathogens in some vegetables. An analytical method was developed to determine mandipropamid residues in agricultural commodities using high-performance liquid chromatography (HPLC) and liquid chromatography/mass spectrometry (LC/MS). Mandipropamid was extracted with methanol from grape, tomato, green pepper, Chinese cabbage and potato samples. The extract was diluted with saturated sodium chloride solution and distilled water, and dichloromethane partition was followed to recover the mandipropamid from the aqueous phase. Florisil column chromatography was employed to further remove interfering co-extractives prior to HPLC analysis. Reverse-phased HPLC was successfully applied to determine mandipropamid in sample extracts with the detection at its ${\lambda}_{max}$ (223 nm). Overall recoveries of mandipropamid from fortified samples averaged $99.8{\pm}1.7$ (n=6), $89.3{\pm}5.3$ (n=6), $98.7{\pm}2.2$ (n=6), $99.7{\pm}6.8$ (n=6) and $91.1{\pm}3.1$ (n=6) for grape, tomato, green pepper, Chinese cabbage and potato, respectively. Limit of quantification of the method was 0.02~0.04 mg/kg for all samples. A LC/mass spectrometry with selected-ion monitoring was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to determine the terminal residue of mandipropamid in agricultural commodities.

Keywords

mandipropamid;fungicide;residue;agricultural commodity

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