Colloids and Surfaces A: Physicochem. Eng. Aspects 465 (2015) 137–146
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Colloids and Surfaces A: Physicochemical and
Engineering Aspects
journa l h om epage: www.elsevier.com/locate/colsurfa
Physicochemical and morphological properties of size-controlled
chitosan–tripolyphosphate nanoparticles
John Antoniou
a
, Fei Liu
a
, Hamid Majeed
a
, Jing Qi
a
, Wallace Yokoyama
b
, Fang Zhong
a,∗
a
Key Laboratory of Food Colloids and Biotechnology, Ministry of Education, School of Food Science and Technology, Jiangnan University, Wuxi 214122,
PR China
b
Processed Foods Research Unit, Western Regional Research Center, ARS, USDA, Albany, CA 94710, United States
h i g h l i g h t s
•
Chitosan–tripolyphosphate nanopar-
ticles were prepared through ionic-
crosslinking.
•
Control of particle size by selecting
appropriate conditions.
•
Influence of initial pH and salinity
of chitosan solution on nanoparticles
formation.
•
Separation of aggregates from
nanoparticles by centrifugation.
•
Ultra-sonication reduced particle size
but caused fragmentation on their
structure.
g r a p h i c a l a b s t r a c t
a r t i c l e i n f o
Article history:
Received 17 June 2014
Received in revised form 9 October 2014
Accepted 23 October 2014
Available online 30 October 2014
Keywords:
Chitosan nanoparticles
Ionic crosslinking
Ionic strength
Particle size
Morphology
Ultra-sonication
a b s t r a c t
Chitosan–tripolyphosphate nanoparticles have been extensively studied during the last decade because
of their numerous applications. In this study, we describe conditions to optimize chitosan nanoparticles
as potential nano-fillers in edible films. The ionic cross-linking between the cationic amino groups on the
chitosan (CS) chain and the anionic phosphate groups of sodium tripolyphosphate (TPP) was verified via
FTIR. Particle size, polydispersity index (PDI) and surface -potential were controlled by chitosan’s Mw
and concentration, CS:TPP mass ratio, and external conditions such as pH and salinity of the initial chi-
tosan solution. Post-processing methods such as centrifugation and ultra-sonication were used to further
control particle size. We show that particle size can be controlled by selecting appropriate conditions.
Particles with sizes below 120 nm were produced at different CS:TPP mass ratios depending on the CS
concentration. Dilute NaCl was the optimal solution ionic composition that decreased the size by 25% and
also resulted in a narrow particle size distribution. We show using UV–vis spectrophotometry that parti-
cles of different size, separated by centrifugation had different phosphorus content. Ultra-sonication can
be used to reduce the size by 50% but long time caused fragmentation of the nanoparticles. Transmission
electron microscopy (TEM) revealed the differences in the morphology of chitosan nanoparticles under
various fabrication conditions.
© 2014 Elsevier B.V. All rights reserved.
∗
Corresponding author. Tel.: +86 510 85328307.
E-mail address: fzhong@jiangnan.edu.cn (F. Zhong).
1. Introduction
Chitosan (CS) is obtained by the deacetylation of the naturally
occurring polysaccharide chitin, one of the most abundant biopoly-
mers in nature. It is composed of -(1-4)-linked d-glucosamine and
N-acetyl-d-glucosamine units [1]. The degree of deacetylation (DD)
http://dx.doi.org/10.1016/j.colsurfa.2014.10.040
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