The separation and identification of organic acids in citrus by-products are critical for evaluating their nutritional and industrial potential. Various techniques focusing on precision, efficiency, and scalability have been developed to achieve this. A high-performance liquid chromatographic (HPLC) separation method with photo-diode array detection has been developed for the simultaneous determination of organic acids and phenolic compounds in juices and drinks. Gas chromatography (GC), often combined with mass spectrometry (GC-MS), provides enhanced identification capabilities for volatile organic acids. Ion chromatography (IC) is another reliable method for quantifying organic acids in citrus by-products. Pre-treatment processes of filtration, centrifugation, and derivatization are critical to improve the accuracy of these techniques. These methods enable the characterization of organic acids for applications in food, pharmaceuticals, and agricultural industries, contributing to the sustainable use of citrus processing residues.