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Column Comparison for the Separation of Ferimzone Z and E Stereoisomers and Development of Trace Residue Analysis Method in Brown Rice Using HPLC-MS/MS

컬럼 비교를 통한 Ferimzone Z 및 E 입체 이성질체의 물질 분리 및 HPLC-MS/MS를 활용한 현미 중 미량잔류분석법 개발

  • Mun-Ju Jeong (Department of Applied Bioscience, Dong-A University) ;
  • So-Hee Kim (Department of Applied Bioscience, Dong-A University) ;
  • Hye-Ran Eun (Department of Applied Bioscience, Dong-A University) ;
  • Ye-Jin Lee (Department of Applied Bioscience, Dong-A University) ;
  • Su-Min Kim (Department of Applied Bioscience, Dong-A University) ;
  • Jae-Woon Baek (Department of Applied Bioscience, Dong-A University) ;
  • Yoon-Hee Lee (Department of Applied Bioscience, Dong-A University) ;
  • Yongho Shin (Department of Applied Bioscience, Dong-A University)
  • 정문주 (동아대학교 생명자원과학대학 응용생명과학과) ;
  • 김소희 (동아대학교 생명자원과학대학 응용생명과학과) ;
  • 은혜란 (동아대학교 생명자원과학대학 응용생명과학과) ;
  • 이예진 (동아대학교 생명자원과학대학 응용생명과학과) ;
  • 김수민 (동아대학교 생명자원과학대학 응용생명과학과) ;
  • 백재운 (동아대학교 생명자원과학대학 응용생명과학과) ;
  • 이윤희 (동아대학교 생명자원과학대학 응용생명과학과) ;
  • 신용호 (동아대학교 생명자원과학대학 응용생명과학과)
  • Received : 2023.08.09
  • Accepted : 2023.08.30
  • Published : 2023.09.30

Abstract

Ferimzone Z is a fungicide for effectively controlling rice blast. Under light irradiation conditions, it undergoes a rapid conversion to its E-stereoisomer. Given the importance of isomers in risk assessments of residues in crops, an analytical method was developed for individual isomer quantification. A comparative analysis performed using two columns in HPLC-MS/MS demonstrated that the isomers were successfully separated using the Cadenza column. For the brown rice sample preparation, 5 g of the homogenized sample was saturated with 7 mL of water. The sample was then extracted with a 10 mL mixed solvent of acetonitrile and ethyl acetate (1:1, v/v) that contained 0.1% formic acid, and it was subsequently partitioned with magnesium sulfate and sodium chloride. The upper layer was purified using dSPE containing C18 and PSA sorbents. The established method was subjected to method validation, and it showed recovery rates of 90.6-98.8% (RSD ≤ 3.9%) at concentrations of 0.01, 0.1, 2 mg/kg, with a soft matrix effect (%ME) ranging from -3.1% to +6.5%. This method can be employed in monitoring studies of brown rice to determine the conversion ratio from the Z isomers to the E isomers.

Keywords

Acknowledgement

This study was carried out with the support of "Cooperative Research Program for Agriculture Science and Technology Development (Project No. PJ017000)", Rural Development Administration, Republic of Korea.

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