<p>This study investigated the sequential extraction of polyphenols and carotenoids from carrots (<i>Daucus carota.</i> L) using pH-responsive Switchable Deep Eutectic Solvents (SDESs) comprising Generally Recognized as Safe (GRAS) substances. DL-Menthol:octanoic acid (1:1 molar ratio, SDES A) and octanoic acid:decanoic acid (1:1 molar ratio, SDES B) were selected for extraction studies after preliminary screening. For both SDESs, Response Surface Methodology paired with Box-Behnken design was used to maximize the extraction yields for both total carotenoid content (TCC) and total polyphenol content (TPC). Maximum TCC extraction yields of 1.33 ± 0.05&#xa0;mg&#xa0;g⁻¹ and 1.50 ± 0.07&#xa0;mg&#xa0;g⁻¹ were obtained using the hydrophobic phases for SDES A and SDES B, respectively. TPC obtained using the hydrophilic phase SDES B under optimal conditions (0.39 ± 0.01&#xa0;mg&#xa0;g⁻¹) was significantly higher than with SDES A (0.31 ± 0.01&#xa0;mg&#xa0;g⁻¹). Sequential extraction of carotenoids using SDES B showed no significant difference in extraction efficiency compared to performing each extraction separately. The addition of citric acid, required for SDES phase separation, increased the antioxidant activity of aqueous extracts by approximately 2.5%. Overall, this study demonstrated the feasibility of a novel approach using a SDES for the sequential extraction of both hydrophilic and hydrophobic bioactive compounds from natural sources as an effective alternative to separate conventional extractions using organic solvents. Moreover, the SDES extracts have potential for utilization in the formulation of active food packaging, functional foods, and other consumer products as they are comprised of GRAS components.</p>