The apparent average molar masses (M w,app ) and apparent average radii of gyration (R g,app ) of native tapioca starch and fractions were determined using asymmetrical flow field flow fractionation (AF4) coupled with multi-angle light scattering and RI detectors (AF4/MALS/RI). AM-type (Fraction A) and AP-type (Fraction B) were chemically separated from native tapioca starch. Native tapioca starch and Fractions (A and B) were dissolved in 1 M KSCN using a high pressure microwave vessel. The effect of varying cross flow rates at a fixed channel flow rate upon the M w,app and R g,app distributions of native tapioca starch and Fractions (A and B) were investigated. The average M w,app values for native tapioca starch, Fraction (A) and Fraction (B) were 59 Â 10 6 , 2.1 Â 10 6 and 19 Â 10 6 g/mol, respectively, with average R g,app values of 165, 73 and 87 nm, respectively. Hydrodynamic radii (R h ) values for native tapioca starch and fractions were determined directly from AF4 experimental parameters.