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[Determination of fipronil and its metabolites in eggs using dispersive- solid phase extraction and gas
Jige Li1, Lanyun Fang1, Yufei Wang1
1Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals of Zhejiang Province, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010, China.
Objective:
To develop a method for determination of fipronil and its metabolites in eggs by gas chromatography-tandem mass spectrometry(GC-MS/MS)cleaned with dispersive-solid phase extraction(D-SPE).
Methods:
Orthogonal array design with OA16(4~4) matrices was used to optimize the efficiency of D-SPE. The targets were extracted from samples with acetonitrile, and followed by D-SPE cleanup. The extracts were analyzed by GC-MS/MS, and quantified by internal standard method with matrix correction.
Results:
The calibration curves showed good linearity in the range of 1.0-250.0 μg/L. The correlation coefficients were larger than 0.99.The average recoveries spiked in eggs at the levels of 2 μg/kg, 4 μg/kg and 20 μg/kg were between 87.1% and 125.0%(n=6), and the relative standard deviations were less than 10%. The limits of determination were between 0.1 and 0.4 μg/kg, and the limits of quantitation were between 0.3 and 1.2 μg/kg.
Conclusion:
The method possesses low background, high sensitivity. It can be applied to determine the residues of fipronil and its metabolites in eggs.
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