Solvent evaporation microencapsulation process
an inner aqueous phase was
made by dissolving an appropriate
amount ofPVA 2( inner aqueous phase)
dependent on the required particle size
(2% w/v for 50–100 and 100–250, and
6% w/v for 250–500 micrometer) in de-
ionized water
To initiate encapsulation, the aqueous
phase was added into the organic
phase, followed by 2 minutes with
gentle shaking by hand to make a
Water-in Oil (W/O) emulsion
(5%w/w+DCM))
After 30minutes, an additional 100mL
of 0.5% w/w PVA solution was added
to further stabilize and solidify the
microcapsules
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After the PVA was dissolved fully, ferrous
ammonium sulfate was dissolved to
The oil phase was obtained by dissolving
5% w/w PMMA in dichloromethane
make a 0.07M ferrous ammonium
(DCM).
solution (as the inner aqueous phase).
with continuous agitation by an RW-16
basic overhead mechanical stirrer at
speeds ranging from 100 rpm to 600
Each W/O emulsion was then poured
rpm (dependent on the desired particle
into 2% w/w PVA solution (outer
size; 200 rpm for microcapsules of 250–
aqueous phase),
500 mm; 600 rpm for microcapsules of
50–100 mm) to form the final
water/oil/water (W/O/W) emulsions.
After microencapsulation, each mixture
was centrifuged at 5000 rpm for
5minutes. All microcapsules were oven dried (60 C)
and weighed before measuring the
The microcapsules were then washed percentage encapsulation efficiency
with de-ionized water three times to
(%EE).
remove the non-encapsulated ferrous
ammonium complex and residual PVA
GAMACHU D.(B.PHARM) AAU 1
 Bead preparation: surface polymerization
process
Briefly, 0.5 g of benzoyl peroxide
(as the initiator) was added to
10mLmethylmethacrylate
(MMA, liquid) and stirred until
fully dissolved (as the organic
phase).
.
The catalyst, 0.2mL 4,N,N-
trimethylaniline was then added
using a transfer pipette, with
continued gentle agitation, to
make a W/O emulsion
The PMMA beads were then
washed with de-ionized water
three times to remove the non-
encapsulated ferrous
ammonium complex and
residual PVA.
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Simultaneously, the 0.07M ferrous
ammonium aqueous phase was
prepared with 6% w/w PVA.
A low agitation speed (<150 rpm)
was maintained to ensure that the
W/O droplets stayed at the surface
of the solution for the
polymerization procedure to occur
(no higher than 150 rpm).
Unlike solvent evaporation
microencapsulation, a wide range
(250 mm to 4mm in diameter) of
PMMA beads can be obtained from
a single batch using the surface
polymerization process.
GAMACHU D.(B.PHARM) AAU
The two phases were combined
with gentle agitation using a plastic
rod (1:10, aqueous: organic).
After the beads were formed, the
whole mixture was agitated at 200
rpm for another 30 minutes to
further stabilize and solidify the
PMMA beads.
All PMMA beads were then dried in
an oven overnight at 60 C.
After drying, the PMMA beads were
sieved and separated using US
standard sieves (three size ranges:
0.5–1, 1–2, and 2–3mm) and
weighed before measuring the %EE.
2