Pectin and mucilage are polysaccharides from the cactus Opuntia ficus-indica, which are also known as hydrocolloids, with useful properties in industries such as food, pharmaceuticals, and construction, among others. In the present work, cactus hydrocolloids were hydrolyzed characterized using two techniques: first, thin-layer chromatography, to identify the monosaccharides present in the sample, followed by the phenol–sulfuric acid method to determine the monosaccharide content. The hydrolyzing method allowed us to reduce the processing time to 180 min and, considering the identification and quantification procedures, the proposed methodology is much simpler and more cost-effective compared to other methods, such as high-performance liquid chromatography (HPLC), nuclear magnetic resonance (NMR), and mass spectrometry. The analysis of the results revealed that the maximum concentration of monosaccharides was obtained after hydrolyzing for 90 min. Under such conditions, with pectin being the main component contained in the cactus hydrocolloids analyzed here, galacturonic acid was found in the largest quantities.