A, Q-Sepharose chromatography. Fractions eluted
from the column were assayed for DBE activity using pullulan (○) or
amylopectin (▪) as a substrate. Products of the amylopectin reaction
were complexed with iodine, and the change in
A550 value relative to untreated substrate
was plotted (▵). Activity units for the amylopectin digestion are
microgram maltose equivalents produced after a 2-h incubation of
substrate with 100 μL of protein fraction. Activity units for the
pullulan digestion are microgram maltotriose equivalents produced after
a 2-h incubation of the substrate with 50 μL of the protein fraction.
Fractions with DBE activity were subjected to immunoblot analysis with
anti-ZPU1 or anti-SU1 antiserum, as indicated (right-hand panels). B,
Gel-filtration chromatography. The peak fractions of pullulanase-type
activity from Q-Sepharose columns were pooled, concentrated, and
applied to a Sephacryl S-200 superfine gel-permeation column. DBE
activity in the fractions eluted from this column was assayed using
pullulan as the substrate; activity units are as described for A.
Fractions were also assayed for the presence of ZPU1 by immunoblot
analysis (right-hand panel). C, Mono-Q chromatography. The peak
fractions (7–11) of pullulanase-type activity from the Sephacryl S-200
column were pooled, concentrated, and applied to a Pharmacia
fast-protein liquid chromatography Mono-Q column. DBE activity in
fractions eluted from this column was assayed using pullulan as the
substrate; activity units are as described for A. Fractions were
assayed for the presence of ZPU1 in immunoblots (right-hand panels). D,
Affinity chromatography. The peak fractions of pullulanase-type
activity from Q-Sepharose columns were pooled, concentrated, and
applied to a column containing epoxy-activated Sepharose conjugated
with cyclohexa-amylose. DBE activity in the four fractions eluted from
this column was assayed using pullulan as the substrate; activity units
are as described for A. Proteins from two of the fractions were
separated by SDS-PAGE and the gel was silver stained; a duplicate gel
was subjected to immunoblot analysis with anti-ZPU1 (right-hand
panels).