This research extracted phenolics and terpenoids from Abelmoschus sagittifolius (Kurz) Merr roots using
natural deep eutectic solvent-based novel extraction techniques. Twelve
natural deep eutectic solvents (NADESs) were produced for recovering
phenolics and terpenoids. Citric acid/glucose and lactic acid/glucose,
with a molar ratio of 2:1, were determined as the most appropriate
NADESs for extracting phenolics and terpenoids, respectively. Afterward,
the proper conditions for NADES-based ultrasonic-assisted and microwave-assisted
extraction were investigated. Then, the time and liquid-to-solid ratios
of ultrasonic- and microwave-combined extraction methods and the sequence
of ultrasound and microwave treatments were examined. The conditions
of ultrasonic-assisted extraction were 40 mL/g liquid-to-solid ratio,
40% water content, 30°C, 5 min, and 600 W ultrasonic power for
the highest terpenoid recovery at 69 ± 2 mg UA/g dw, while 150
W ultrasonic power was suitable for phenolic recovery at 9.56 ±
0.17 mg GAE/g dw. The conditions of microwave-assisted extraction
were 50 mL/g liquid-to-solid ratio, 20% water content, 400 W microwave
power, and 2 min to acquire the highest phenolics and terpenoids at
22.13 ± 0.75 mg GAE/g dw and 90 ± 1 mg UA/g dw, respectively.
Under appropriate conditions, the biological activities, phenolic
content, and terpenoid content of obtained extracts from four extraction
methods, including ultrasonic-assisted, microwave-assisted, ultrasonic–microwave-assisted,
and microwave–ultrasonic-assisted extraction, were compared
to select the most proper method. The conditions of ultrasonic–microwave-assisted
extraction were 40 mL/g liquid-to-solid ratio, 5 min sonication, and
1 min microwave irradiation to obtain the highest phenolic and terpenoid
contents (27.07 ± 0.27 mg GAE/g dw and 111 ± 3 mg UA/g dw,
respectively). Ultrasonic–microwave-assisted extraction showed
the highest phenolic content, terpenoid content, and biological activities
among the four extraction techniques. The changes in the surface morphology
were determined using scanning electron microscopy. This study demonstrated
that ultrasonic–microwave-assisted extraction was an effective
and sustainable method in food and pharmaceutical industries for recovering
phenolics and terpenoids from Abelmoschus sagittifolius (Kurz) Merr.