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The Effects of Surfactant Polysorbate-

80 and NaCl Electrolyte Concentrations


on the Size Stability of Nanochitosan
during Storage
Annisa Primaningtyas, Wiratni Budhijanto,
M. Fahrurrozi, Yuni Kusumastuti
BACKGROUND

A preservation
agent

6.5 million Perishable food


tonnes per year
nanochitosan
Surfactant modification NaCl effect
(Polysorbate-80)
unstable particle
size
Nanochitosan Formation
Ionic Gelation Method

4
Crosslinking Reaction

Mi, et. al. 1999


Ionic Gelation Process

• Spontaneous reaction
• Occur in mild condition

• Has low level of stability when stored in a


certain time due to swelling or agglomeration
• has a wide particle size distribution
MATERIALS
Chitosan

• Characteristics = antimicrobial and non-toxic


• Has been widely used as a food preservative and packaging
material
Surfactant (Polysorbate-80)
Hydrophobic
group

• Polyoxyethylene 20 sorbitan monooleate H H

• nonionic surfactant
• non toxic
• stability agent O O

O OH
O

O
O

HO

HO

Hydrophilic group
Sodium Tripolyphosphate (TPP)

• multivalent polyanion
• non toxic, easy handling
•Cross-linker
• to form nanochitosan particles by ionic
cross-linking between chitosan chains.
METHODS
Acetic acid Chitosan
1% 0,2%
Chitosan Surfactant
Aquadest Acidic solution dispersion solution:
0.05%
0.1%
Time: Nanochitosan- 0.2%
Nanochitosan Chitosan-
Day 0 NaCl
dispersion surfactant
Day 14 dispersion dispersion
Day 28 NaCl
(by 0% TPP solution
Particle size 3% 0,84 mg/mL
Analyzer) Chitosan : TPP = 5:2 (v/v)
10
RESULTS
NaCl 0% NaCl 3%
600 500
500
particle size, nm

400

particle size, nm
400 0.05%
0.05% 300
300 0.1%
0.1% 200
200
0.2%
100 0.2% 100
0 0
0 14 28 0 14 28
time, days time, days

• NaCl 0%
– Range particle size = 345.6 to 515.3 nm not visually different
• NaCl 3%
– Range particle size = 175.0 to 391.8 nm
ANOVA
ANOVA
Sum of degree of mean
source of variation F0 calc F0 table Information
Squares freedom square

time (A) 13259.03 2 6629.517 3.93 3.55 significant

polysorbate-80
1228967 2 614.4836 0.36 3.55
concentrations (B)

NaCl concentrations (C) 255547.1 1 255547.1 151.61 4.41 significant

AB 5742.696 4 1435.674 0.85 2.93


AC 13722.93 2 6861.465 4.07 3.55 significant
BC 2058.034 2 1029.017 0.61 3.55
ABC 8602.543 4 2150.636 1.27 2.93
Error 30338.61 18 1685.478
Total 330499.9 35
Particle Size Distribution: NaCl 0%
50 50
Day 0 Day 14 50
Day 28
40 40 40
frequency, %

frequency, %
frequency, %
30 30 30
0.05% 0.05% 0.05%
20 0.1% 20 0.1% 20 0.1%
0.2% 0.2% 0.2%
10 10 10

0 0 0
0 500 1000 1500 2000 2500 3000 0 500 1000 1500 2000 2500 3000 0 500 1000 1500 2000 2500 3000
average particle size, nm average particle size, nm average particle size, nm

• On day 14, the influence of surfactant can be seen from narrowed


particle size distribution in the range of 250-800 nm.
• On day 28, a bimodal distribution pattern indicated particle
agglomeration mechanism.
Particle Size Distribution: NaCl 3%
50 Day 0 50 Day 14 50
Day 28
40 40 40

frequency, %
frequency, %

frequency, %
30 30 30
0.05% 0.05% 0.05%
20 0.1% 20 0.1% 20 0.1%
0.2% 0.2% 0.2%
10 10 10

0
0 0
0 500 1000 1500 2000 2500 3000
0 500 1000 1500 2000 2500 3000 0 500 1000 1500 2000 2500 3000
average particle size, nm average particle size, nm average particle size, nm

• the particle size distributions during storage tend to be


narrowed during 28 days of storage.
• The NaCl addition reduced nanoparticles agglomeration
which indicated by particle size reduction.
Particle Size Distribution: Overtime Storage
35 NaCl 0% 35 NaCl 3%
day 0 30 day 0
30

frequency, %
day 3 25 day 3
25
day 7
frequency, %
20 day 7
20
day 14 15 day 14
15
day 28 10 day 28
10
day 141 5 day 141
5
0
0
0 500 1000 1500 2000 2500 3000
0 500 1000 1500 2000 2500 3000
average particle size, nm average particle size, nm

• NaCl 0%
– During 141 days, the agglomeration of particle occurred. It was indicated by wide
unimodal size distributions
• NaCl 3%
– A very narrow particle size distribution can be seen on day 14, 28, and 141
– the addition of a 3% NaCl stabilized and narrowed particle size distributions up to
141 days of storage.
Nanochitosan Dispersions

NaCl 0% NaCl 3%
CONCLUSIONS

• The storage time and NaCl concentration have


much influences on the stability of nanoparticle
sizes
• The NaCl addition had significant effect to
prolong the stability of nanochitosan dispersions.
Thank You
This research is granted by: MP3EI Project

Contact Person:
Annisa Primaningtyas
annisa.p@mail.ugm.ac.id

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