An innovative approach for extracting and separating analytes consecutively from complex matrixes was introduced for the first time. The approach involves applying centrifugal force to a novel circular chip to expedite the process of microsolid phase extraction and centrifugal acceleration thin-layer chromatography, followed by red−green−blue (RGB) analysis as a simple, fast, and in situ detection method. Furthermore, the natural product of rice husk was utilized to create a sorbent with great adsorption capabilities. In this method, curcumin and phenazopyridine were employed as model drugs. The one-variable-at-a-time (OVAT) method was used to study the factors that affect the extraction and separation. Under the optimized conditions, a good relationship was observed between the |R| + |B| intensity and the concentration of analytes within the range of 1.0−10.0 μg/ mL (R 2 = 0.9903) for curcumin and 0.1−7.5 μg/mL (R 2 = 0.9933) for phenazopyridine in urine samples. Intra-and interday RSDs% (n = 3) were obtained at less than 5.6 and 7.1%, respectively. In urine samples, the limit of detection values was 0.75 μg/mL for curcumin and 0.05 μg/mL for phenazopyridine, and relative recovery values were in the acceptable range of 85.0−100.2%. The suggested approach has the appropriate sensitivity, good accuracy, and acceptable applicability to determine curcumin and phenazopyridine in complicated matrices.