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Background: Consistent toxicological evidence indicate that phthalates can cause adverse effects on human health. The concern over phthalate pollution and exposure has been emphasized in recent years. Therefore, the sensitive, reliable, and rapid detection of phthalates in water is of great importance. Objective: In this study, dispersive liquid–liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) combined with HPLC-UV detection was established and applied in the preconcentration and detection of 15 phthalates in drinking and river water samples. Methods: A mixture of acetonitrile (dispersant) and 1-dodecanol (extractant) was injected into water samples, which had been added with sodium chloride. The cloudy solution was formed by hand-shaking. After centrifugation, the sample solution was cooled in a refrigerator, and the solidified organic droplet was collected. It …