Determination of fipronil by solid-phase microextraction and gas chromatography–mass spectrometry

A method for the determination of trace amounts of the insecticide fipronil was developed using solid-phase microextraction–gas chromatography–mass spectrometry and selected ion monitoring. Fipronil was extracted with a fused-silica fiber coated with 85 μm polyacrylate. The effects of pH, ionic strength, sample volume, extraction and desorption times as well as the extraction temperature were studied. Lindane was used as an internal standard. The linear concentration range of application was 0.3–100 ng ml−1 of fipronil, with a relative standard deviation of 9.5% (for a level of 50 ng ml−1) and a detection limit of 0.08 ng ml−1. The method was applied to check the eventual existence of fipronil above this limit in water and soil samples from Granada (Spain) as well as in human urine samples. The method validation was completed with spiked matrix samples. The method can be applied as a monitoring tool for water, soil and urine, in the investigation of environmental and occupational exposure to fipronil.