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As the world population continues to grow, so does the pollution of water resources. It is, therefore, important to identify ways of reducing pollution as part of our effort to significantly increase the supply of clean and safer water. In this study, the efficiency of ultrasound-assisted dispersive liquid–liquid microextraction (UA-DLLME) as a fast, economical, and simple method for extraction malachite green (MG) and rhodamine B (RB) dyes from water samples is investigated. In optimal conditions, the linear dynamic range (LDR) for RB and MG is 7.5–1500 ng mL−1 and 12–1000 ng mL−1, respectively. The limit of detection (LOD) is 1.45 ng mL−1 and 2.73 ng mL−1, and limit of quantification (LOQ) is 4.83 ng mL−1 and 9.10 ng mL−1 for RB and MG, respectively. Extraction efficiency is obtained in the range of 95.53–99.60%. The relative standard deviations (RSD) in real water and wastewater samples are less than 3.5. The developed method is used successfully in the determination of RB and MG dyes from water samples and there are satisfactory results.

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