• Korean Journal of Food Science and Technology
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• v.51 no.4
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• pp.316-323
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• 2019

It is difficult to analyze pymetrozine in citrus fruits using the hydromatrix method because of its low efficiency of purification and overlap of matrix and pymetrozine peaks. Liquid-liquid extraction can analyze pymetrozine in citrus fruits using dichloromethane. Since low pH interferes with the extraction of pymetrozine, the extracts of citrus fruits were maintained over pH 7.0 by adding borax buffer and 1 N NaOH in the improved method. According to the improved method, citrus fruits (such as lemon, lime, orange, tangerine, and grapefruit) were extracted and purified for HPLC-photo diode array analysis. The results of validation were as follows: $4.360{\mu}g/kg$ of limit of detection, $14.533{\mu}g/kg$ of limit of quantitation, and 0.007 mg/kg of method quantitative limit. Citrus fruits spiked with pymetrozine showed a recovery range from 71.8 to 83.7% and a coefficient of variation below 6%. Thus, the improved method can efficiently analyze pymetrozine in citrus fruits.

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