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Microwave-assisted extraction of pyrethroid insecticides from semi permeable membrane devices (SPMDs) used to indoor air monitoring
Francesc A. Esteve-Turrillas, Agust´ın Pastor, Miguel de la Guardia

Abstract：
A rapid and environmentally friendly methodology was developed for the extraction of pyrethroid insecticides from semi permeable membrane devices (SPMDs), in which they were preconcentrated in gas phase. The method was based on gas chromatography mass–mass spectrometry determination after a microwave-assisted extraction, in front of the widely employed dialysis method. SPMDs were extracted twice with 30mL hexane:acetone, irradiated with 250Wpower output, until 90 ◦C in 10 min, this temperature being held for another 10 min. Clean-up of the extracts was performed by acetonitrile–hexane partitioning and solid-phase extraction (SPE) with a combined cartridge of 2 g basic-alumina, deactivated with 5% water, and 500 mg C18.

Pyrethroids investigated were Allethrin, Prallethrin, Tetramethrin, Bifenthrin, Phenothrin,
-Cyhalothrin, Permethrin, Cyfluthrin, Cypermethrin,Flucythrinate, Esfenvalerate, Fluvalinate and Deltamethrin. The main pyrethroid synergist compound, Pyperonyl Butoxide, was also studied. Limit of detection values ranging from 0.3 to 0.9 ng/SPMD and repeatability data, as relative standard deviation, from 2.9 to 9.4%, were achieved. Pyrethroid recoveries, for spiked SPMDs, with 100 ng of each one of the pyrethroids evaluated, were from 61±8 to 103±7% for microwaveassisted
extraction, versus 54±4 to 104±3% for dialysis reference method. Substantial reduction of solvent consumed (from 400 to 60 mL) and
analysis time (from 48 to 1 h) was achieved by using the developed procedure.

High concentration levels of pyrethroid compounds, from 0.14 to 7.3 ug/SPMD, were found in indoor air after 2 h of a standard application.


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