Establishment of Analytical Method for Pymetrozine Residues in Crops Using Liquid-Liquid Extraction(LLE)

액-액 분배법을 활용한 작물 중 pymetrozine의 잔류분석법 확립

  • Yoon, Ji-Young (Department of Bio-Environmental Chemistry, Chungnam National University) ;
  • Moon, Hye-Ree (Department of Bio-Environmental Chemistry, Chungnam National University) ;
  • Park, Jae-Hun (Department of Bio-Environmental Chemistry, Chungnam National University) ;
  • Han, Ye-Hoon (Syngenta, Korea Ltd.) ;
  • Lee, Kyu-Seung (Department of Bio-Environmental Chemistry, Chungnam National University)
  • 윤지영 (충남대학교 농업생명과학대학 생물환경화학과) ;
  • 문혜리 (충남대학교 농업생명과학대학 생물환경화학과) ;
  • 박재훈 (충남대학교 농업생명과학대학 생물환경화학과) ;
  • 한예훈 (신젠타 코리아(주)) ;
  • 이규승 (충남대학교 농업생명과학대학 생물환경화학과)
  • Received : 2013.05.14
  • Accepted : 2013.06.19
  • Published : 2013.08.30


Polar pesticides like pymetrozine (log $P_{ow}$: -0.18) are known to be difficult to analyze. The analytical method of pymetrozine using hydromatrix included in the official method of KFDA was uncommon and provided ambiguous evidence to confirm both the identity and the quantity. Therefore, precise single residue analytical method was developed in representative crops for using liquid-liquid extraction (LLE). The pymetrozine residue was extracted with methanol from 11 representative crops which comprised apple, blueberry, broccoli, cabbage, cherry, crown daisy, hulled rice, Korean cabbage, potato, rice and watermelon. The extract was purified serially by liquid-liquid extraction (LLE) and silica solid phase extraction (SPE). For rice and hulled rice samples, n-hexane partition was additionally adopted to remove nonpolar interferences, mainly lipids. The residue levels were analyzed by HPLC with DAD, using $C_8$ column. LOQ (limit of quantitation) of pymetroizinie was 1 ng (S/N > 10) and MQL (method quantitation limit) was 0.01 mg/kg. Mean recoveries from 11 crop samples fortified at three levels (MQL, 10 ${\times}$ MQL and 50 ${\times}$ MQL) in triplicate were in the range of 83.1~98.5% with coefficients of variation (CV) of less than 10%, regardless of sample type, which satisfies the criteria of KFDA. The method established in this study could be applied to most of crops as an official and general method for analysis of pymetrozine residue.


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