Ultrasonic assisted headspace single drop micro-extraction and gas chromatography with nitrogen-phosphorus detector for determination of organophosphorus pesticides in soil

This work describes optimization of headspace single drop micro-extraction for extraction of five organophosphorus pesticides; thionazin, sulfotep, dimethoate, disulfoton and parathion in soil. Ultrasound has also been used successfully to improve and accelerate the extraction of the analytes from the sample. The optimized extraction performance was obtained when the experimental parameters were set as follows; 3.0 μL of octanol as extraction solvent, high ionic strength (20% sodium chloride), 1:1 (w/v) sample dilution with water, extraction temperature at 60 °C for 30 min; applying ultrasound and without any pH adjustment. The optimized method was linear over the calibration range (5–200 and 10–300 for different analytes) with limits of detection of 0.1–2.0 ng g−1. The enrichment factor for OPPs was 1.4–12.7 and the method was also reproducible with the relative standard deviations (RSD%) of 2.1–6.9%.

Figure optionsDownload as PowerPoint slideHighlights
► A 2 g portion of soil sample was enough for trace analysis of OPPs at ng g−1 level.
► Despite low volatility, OPPs could be headspace extracted under mild conditions.
► Ultrasonic agitation showed to provide better results than magnetic stirring.