Marine organisms use mycosporine-like amino acids (MAAs) as biological sunscreens for the protection from damaging ultraviolet (UV) radiation and the prevention of oxidative stress. MAAs have been discovered in many different marine and freshwater species including cyanobacteria, fungi, and algae, but also in animals like cnidarian and fishes. Here, we describe a general method for the isolation and characterization of MAA compounds from red algae and symbiotic dinoflagellates isolated from coral hosts. This method is also suitable for the extraction and analyses of MAAs from a range of other algal and marine biota.