A procedure for the determination of galacturonic acid and the main neutral sugars in pectins involves enzymic hydrolysis followed by methanolysis and h.p.l.c. The usefulness of this method was demonstrated by comparison of the results obtained by (1) methanolysis in methanolic m HCl without enzymic prehydrolysis, (2) methanolysis in methanolic 72% H2SO4 with pretreatment for 3 h with aqueous 72% H2SO4, (3) colorimetric determination of galacturonic acid, and (4) g.l.c. of the alditol acetates of the neutral sugars released by acid hydrolysis under various conditions. © 1990.