Domoic acid was recognized recently to be a marine neurotoxin associated with shellfish harvested or cultured for use as human food. Evidence about the occurrence of domoic acid and its importance to shellfish industries is reviewed. The preparation and certification of two reference materials for the determination of domoic acid, an instrument calibration solution (DACS-1, released by the Marine Analytical Chemistry Standards Program [MACSP] in May, 1989), and a tissue reference material (MUS-1, homogenized soft tissues of Mytilus edulis, released by the MACSP in August, 1989) are described. We believe these are the first certified standards or reference materials to be available for the determination of shellfish toxins, a problem of increasing importance to aquaculturists and the seafood industry, as well as to agencies concerned with the safety of food. The tissue homogenate preparation techniques we have developed and used may be of general interest for the preparation of other tissue reference materials for the determination of other organic compounds, since the sealed, fluid homogenate samples seem acceptably stable without being continuously frozen or refrigerated.