Citrus contains a range of highly beneficial bioactive compounds, such as polyphenols, carotenoids, and vitamins that show antimicrobial and antioxidant properties and help in building the body’s immune system. On consumption or processing, approximately 50% of the fruit remains as inedible waste, which includes peels, seeds, pulp, and segment residues. This waste still consists of substantial quantities of bioactive compounds that cause environmental pollution and are harmful to the ecosystem because of their high biological oxygen demand. In recent years, citrus cultivation and the production of processed foods have become a major agricultural industry. In addition to being a substantial source of economy, it is an ideal and sustainable and renewable resource for obtaining bioactive compounds and co-products for food and pharmaceutical industries. In the present article, the various methods of extraction, conventional and modern, as well as separation and isolation of individual bioactive compounds from the extraction mixture and their determination have been reviewed. This article presents both aspects of extraction methods, i.e., on a small laboratory scale and on an industrial mass scale. These methods and techniques have been extensively and critically reviewed with anticipated future perspectives towards the maximum utilization of the citrus waste.