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Deep eutectic solvents (DES), which have low toxicity and are low cost, biodegradable, and easily synthesized, were used for the extraction of neutral red (NR) dye before its spectrophotometric analysis. DES, containing choline chloride as a hydrogen bond acceptor and phenol as a hydrogen bond donor with a molar ratio of 1:2, was used for the extraction of NR dye from aqueous media. The possible interaction of different DESs with NR was studied using density functional theory (DFT) calculations. Experimentally, a UV-visible spectrophotometer was used for the quantitative analysis. The most important parameters affecting method performance, such as pH, extraction temperature, DES type, its volume, THF volume, sonication time, and centrifugation time, were optimized. The developed method provides exceptional sensitivity in terms of LOD and LOQ, which were 2.2 and 7.3 µg/L respectively. The relative standard deviation was 1.35–1.5% (n = 10), and the pre-concentration factor was 40. The method was found to be linear in the range of 2–300 µg/L (R2 = 0.9967). The method was successfully used for the determination of NR in wastewater samples. Finally, the DES-based method presents operational simplicity, high sensitivity, and rapid determination (<5 min) compared with other analytical procedures. [ABSTRACT FROM AUTHOR]

[Display omitted] • Green chemistry sample preparation concept by means of Deep Eutectic Solvents (DES). • Novel DES based approach for pre-concentration of Niclosamide. • Effective method dedicated to determination of Niclosamide in pharmaceutical and wastewater samples. • Step forward for trace analysis of Niclosamide in environmental samples. The paper presents a simple, but very effective and sensitive spectrophotometric method for trace analysis of Niclosamide based on liquid–liquid microextraction using deep eutectic solvents (DESs) prior to its quantification. Here, different DES systems, such as Choline chloride (ChCl) + Urea, ChCl + Citric acid, ChCl + Ethylene glycol and ChCl + Phenol, were synthesized and evaluated at different molar ratios, selecting ChCl + Phenol 1:2 as an extractive DES system. Optimization studies revealed that best performance were obtained at pH 8 with optimum volume of THF and DES as 0.3 mL and 0.4 mL, respectively. The developed method is characterized by good analytical performance, e.g., a recovery of 99.26% and precision described by RSD value as <2%. The inter-assay precision was 0.51% while intermediate precision was 0.0323%. The method was found linear from 4.8 to 48 µg/L. LOD and LOQ were found as 0.112 and 0.374 µg/L, respectively. The paper presents also examples of the application of the proposed method for the determination of Niclosamide in different pharmaceutical and wastewater samples. This alternative method reveals a better performance in respect to the British pharmacopoeia procedure, providing concurrently ease of operation and simplicity. [ABSTRACT FROM AUTHOR]