A microextraction technique based on ultrasonic emulsification and demulsification was developed for detecting pesticides at trace levels in environmental water samples. In this ultrasound-assisted microextraction (UAME), chloroform was emulsified with an aqueous sample solution containing trace fenitrothion (MEP) by ultrasonic irradiation (48 kHz) for 5 min. The emulsion was then demulsified by ultrasonic irradiation (2.4 MHz) for 10 min. This resulted in phase separation of the water and chloroform without centrifugation. The demulsified chloroform was collected by a microsyringe and submitted to gas chromatography-mass spectrometry. In conventional extraction with mechanical stirring, the extraction recovery (ER) of MEP was strongly dependent on the sample/chloroform volume ratio. However, in UAME, the ER was independent of the volume ratio and the ER was >80 % when the enrichment factor was 40. In UAME, MEP was rapidly extracted into the chloroform because of the large specific surface areas of the small chloroform droplets in the oil-in-water (O/W) emulsion. This gave a high extraction efficiency for MEP. UAME is a simple method requiring only a change in the ultrasound frequency and with no pretreatment steps that could contaminate the sample. The suitability of UAME was demonstrated by application to the detection of trace levels of pesticides in a spiked water sample from a fish tank. Graphical abstract Schematic diagram of the ultrasound-assisted microextraction (UAME) method.
Keywords: Dispersive liquid–liquid extraction; Fenitrothion; Gas chromatography–mass spectrometry; Pesticide analysis; Ultrasound-assisted microextraction (UAME).