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A new sample pretreatment technique, ultrasound-assisted headspace liquid-phase microextraction was developed in this paper.In the technique, the volatile analytes were headspace extracted into a small drop of solvent, which suspended on the bottom of a cone-shaped PCR tube but not at the needle tip of a microsyringe.More solvent can be suspended in the PCR tube due to the larger interfacial tension, thus the analysis sensitivity was significantly improved with the increase of the extractant volume.Moreover, ultrasonic extraction and independent controlling temperature of extractant and sample were performed to enhance the extraction efficiency.