Nanostarch has attracted great attention owing to its
high biocompatibility,
easy availability, low sensitization, small size, and large specific
surface area. However, most well-dispersed spherical nanostarches
are currently produced under chemical surfactants. Here, we use controllable
dynamic high-pressure microfluidization (DHPM) with a nanoprecipitation
method to prepare smooth surface and homogeneous starch nanospheres
(SNSs). Under the microfluidization condition in a homogenization
cycle of ×4 and pressure of 100 MPa, the smallest particle size
(67.1 nm) of SNSs with excellent dispersibility (PDI 0.307) was obtained.
In addition, after DHPM treating, the crystal structure of starch
was damaged. Also, V-type crystallinity was observed after nanoprecipitation,
and side chains in starch were cut as performed in an inside-out mode
to form small starch clusters. Notably, by mechanical forces, the
positions of the OH groups of starch glucan rings were greatly motivated
in the spectra of FTIR, 1H NMR, 13C NMR, and
XPS. They were cross-linked with each other to form new microstructures
of −C–O–C– groups. Furthermore, this should
be highlighted for the importance of pressure and homogenization cycle
conditions in order to prepare bioresource nanomaterials with well-dispersed
properties according to food and nonfood applications like delivery
systems.