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[Display omitted] • A novel, green and environmental benign TC-AALLME-SFDES technique was developed. • Solid DES was used as extraction solvent. • The method was applied for the determination of TCS and APs from water samples. • The green profile of the method was assessed by analytical Eco-Scale and ComplexGAPI. • The method opened up the application of solid DESs in LLME technique. A novel and green microextraction technique, temperature-controlled air-assisted liquid–liquid microextraction based on the solidification of floating deep eutectic solvents (DESs), was developed and applied for the extraction of triclosan and alkylphenols in different environmental waters. Hydrophobic DESs composed of menthol and myristic acid with melting points slightly higher than room temperature (25 ± 2 °C) were prepared and used as extraction solvent. First, the solid DES was transformed into liquid DES while the aqueous sample was heated in a water bath. Then, fine droplets were formed by withdrawing and injecting the mixture of aqueous sample and DES with a 1 mL pipette several times. After extraction, the solidified DES phase was obtained in an ice water bath. And then the analyses were performed by HPLC-UV. The microextraction parameters were investigated by the Plackett-Burman design and central composite design. The analytical parameters of this method were investigated and good linear ranges (0.5/1.0–400 μg/L, R2 ≥ 0.9950), limits of detection (0.1–0.5 μg/L) and precision (≤5.9 %) were obtained. This method was successfully applied for the determination of triclosan and alkylphenols from five water samples with satisfactory recoveries (80.0–104.3 %). Subsequently, the green profile of the method was assessed by analytical Eco-Scale and Complementary Green Analytical Procedure Index. This method has the advantages of simplicity, rapidity, low cost, high sensitivity and green, which expands the application of solid solvents in liquid–liquid microextraction and has a wide application prospect. [ABSTRACT FROM AUTHOR]

• One-step derivatization and TC-VA-LLME-SFDES method was developed. • Hydrophobic DESs were used as both reducing agent and extraction solvent. • Only 2 min was needed for derivatization and extraction process. • The method was applied for analysis of total Fe in water and food samples. • The method opened up the application of solid DESs in LLME technique. In our work, hydrophobic thymol-based deep eutectic solvents (DESs) with strong reducibility, a lower density than water, and a slightly higher melting point than room temperature were synthesized. Based on these solid DESs, one-step derivatization and temperature-controlled vortex-assisted liquid-liquid microextraction based on the solidification of a floating DES (TC-VA-LLME-SFDES) via UV–Vis spectrophotometry for the rapid determination of total iron was developed. The derivatization and TC-VA-LLME were carried out simultaneously by the addition of DES as both the reducing agent and extraction solvent. After optimization, the calibration curve (5–250 μg L−1, R2 = 0.9982), limit of detection (1.5 μg L−1), limit of quantitation (5.0 μg L−1), precision (≤4.0%) and enrichment factor (92) was obtained. This method was applied for the determination of total iron in water and food samples with satisfactory recoveries (85.4–106.2%). One-step derivatization and TC-VA-LLME only required 2 min. Furthermore, this method opened up the application of solid DESs in liquid–liquid microextraction. [ABSTRACT FROM AUTHOR]