Rapid and sensitive determination of pyrethroids indoors using active sampling followed by ultrasound-assisted solvent extraction and gas chromatography

A fast and simple method to analyze pyrethroids as well as other components of frequently used domestic insecticide preparations in indoor air is presented. The proposed method, based on sampling with an adsorbent followed by ultrasound-assisted solvent extraction, was developed with the aim to simplify the traditional extraction methodologies applied up to date to determine pesticides in air. The analytes were retained on a very small amount of adsorbent, which allowed using solely 1 mL of solvent for desorption. The quantification was performed by gas chromatography with microelectron-capture detection (GC–μECD) and gas chromatography coupled to mass spectrometry (GC–MS). The influence of main factors involved in the ultrasound-assisted solvent extraction step (type of adsorbent and type of solvent, solvent volume and extraction time) was studied using an experimental design approach to account for possible factor interactions. The sampling step was studied for two adsorbents (Tenax TA and Florisil), finding that 1 m3 air could be sampled without losses of analytes. In this way, the analysis of pyrethroids in air by the proposed method could be carried out within a total time shorter than an hour, including sampling. Linearity was demonstrated in a wide concentration range. Efficiency of the total sampling–extraction process was studied at several concentration levels (2, 10, 100 and 1000 ng/m3), obtaining quantitative recoveries for all compounds, with good precision (RSD < 10%). Method detection limits were below 1 ng/m3 in air when GC–μECD was employed, and about one order of magnitude higher for GC–MS. In addition, the proposed method was applied to real samples collected in contaminated closed rooms, in which some of the target compounds were determined.