In this work, an ultrasonic-assisted supramolecular based on solidification of floating organic drop microextraction (UA-SM-SFO-ME) was developed as a green method for preconcentration of methadone prior to gas chromatography-mass spectrometry (GC-MS). The supramolecular solvent aggregates containing reverse micelles of 1-dodecanol in tetrahydrofuran (THF) were formed by ultrasonication that subsequently dispersed in the sample solution. Ultrasonic waves caused the fast formation of supramolecular solvent aggregates. In this work, ultrasonication was used in two phases: First phase, the formation of reverse micelles and the second phase, the dispersion of supramolecular solvent in the sample solution. Actually, ultrasonication was basic of this presented work. In order to provide the highest extraction efficiency, the influence of various parameters on the method performance (supramolecular solvent type and volume, disperser solvent condition, pH, extraction time and salt concentration) was investigated. Based on the obtained optimum conditions, the limits of detection (LODs) and the limits of quantitation (LOQs) were obtained 0.5-1.2 µg L and 1.2-2.5 µg L with preconcentration factors in the range of 182-191, in water and biological samples, respectively. Subsequently, the method was assessed for preconcentration of the methadone in human plasma and saliva samples.
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