Synthetic pyrethroid insecticides analysis by gas chromatography/mass spectrometry operated in negative‐ion chemical ionization mode in soil, moss and fish tissue

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Abstract
A gas chromatographic/mass spectrometric method was developed for the simultaneous determination of five synthetic pyrethroid insecticides in soil, moss and fish tissue. These pyrethroids were extracted with hexane‐dichloromethane by ultrasonication and cleaned up on Florisil (soil and moss) and mixed acid/base alumina (fish) columns prior to determination by gas chromatography/negative‐ion chemical ionization mass spectrometry in selected ion monitoring mode. All the pyrethroids were analyzed simultaneously in a single run on a DB5‐MS 15 m capillary column. Recoveries of the pyrethroids from the three matrices at fortification levels of 10, 50 and 100 μg/kg ranged from 80 to 117%. Four determinations were made at each concentration level for each matrix. The practical determination limit of the method was in the range 0.5 to 5 μg/kg depending on the compound. This method was also applied to samples obtained from a contaminated ecosystem.