• The Korean Journal of Pesticide Science
• /
• v.17 no.2
• /
• pp.107-116
• /
• 2013

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.