SUMMARY. Four hundred and ®fty-four subjects with hyperamylasaemia were screened for the presence of macroamylase using polyethylene glycol precipitation (PEG) and the Beckman automated amylase assay based on the hydrolysis of maltotetraose. Twenty-®ve subjects (5´5%) exhibited PEG precipitation values suggestive of macroamylasaemia (MA) (452% loss of original amylase activity). Macroamylasaemia was con®rmed by gel ®ltration chromatography (GFC) in 21/25 subjects, using albumin as a molecular weight marker. Biochemical and clinical details of the 21 subjects identi®ed are presented and discussed. It is recommended that serum exhibiting more than 57% precipitation of the original amylase activity by PEG should be examined by GFC to con®rm or exclude MA.