The sustainable extraction of saponins was investigated using natural deep eutectic solvents (NADESs) combined with ultrasound-assisted extraction. A novel NADES (butyric acid-urea) that was responsive to ionic strength was designed and used as the extractant. Ultrasound treatment and a catalyst ferric chloride with plant cell wall breaking function were applied to improve the extraction efficiency.Since the solubility of the NADES varied significantly with ionic strength, 95% of NADES was readily separated from the water phase after the addition of sodium chloride, while saponins remained in the water phase for easy collection. The reuse capacity of NADES, the eco-friendliness of the extraction method, and the antioxidant activity of the extract were further evaluated.NADES was continuously recovered and used to extract Polygonatum sibiricum powder: the yield of saponins did not decrease after five cycles of recovery and re-extraction. The penalty point on the "Eco-scale" suggested that the extraction method was "green" (i.e. eco-friendly).Compared with ethanol extracts, the NADES extracts showed a higher saponin concentration and antioxidant activity.The study can contribute to the sustainable and green extraction of hydrophilic active substances in the food and pharmaceutical industries.

This work presents a novel and green analytical procedure involving a deep eutectic solvent-based dispersive liquid–liquid microextraction with solidification of floating organic droplets (DES-DLLME-SFOD) followed by HPLC to measure three pyrethroids (bifenthrin, β-cypermethrin, and deltamethrin) in cereal samples. Firstly, a low-density hydrophobic DES was synthesized from thymol and octanoic acid in the molar ratio of 1/4 and this was applied as a green extraction solvent in the DLLME procedure to avoid the use of a toxic extractant. After centrifugation and placing it on an ice bath, it is transformed into a solid phase on the top of the sample solution to reduce the loss of extractant, conducive to convenient collection thereafter. This procedure required the optimal conditions (including the type, proportion, and amount of DES as the extractant, the volume of the dispersant acetonitrile, the amount of salt, and the pH value) to be evaluated. Under optimized variates, the proposed method provided good linearity with a correlation coefficient greater than 0.997 and limits of quantification within the range of 6.6–8.9 μg kg⁻¹. The recoveries of pyrethroids in corn, wheat, barley, and oats were 75.6–87.2%, and the relative standard deviation was less than 3.6%. The method, therefore, offers a green, efficient, and convenient approach for the determination of pesticides in cereals.