The document describes two microencapsulation processes: solvent evaporation and surface polymerization. For solvent evaporation, an aqueous solution containing ferrous ammonium sulfate was emulsified in an oil phase containing PMMA and dichloromethane to form microcapsules between 50-500 micrometers. For surface polymerization, an aqueous solution was emulsified in a monomer solution of methyl methacrylate containing an initiator and catalyst to form larger PMMA beads from 250 micrometers to 4 millimeters through polymerization at the surface of droplets. Both methods produce microcapsules or beads encapsulating ferrous ammonium complexes that are then dried and sieved for analysis.
The document describes two microencapsulation processes: solvent evaporation and surface polymerization. For solvent evaporation, an aqueous solution containing ferrous ammonium sulfate was emulsified in an oil phase containing PMMA and dichloromethane to form microcapsules between 50-500 micrometers. For surface polymerization, an aqueous solution was emulsified in a monomer solution of methyl methacrylate containing an initiator and catalyst to form larger PMMA beads from 250 micrometers to 4 millimeters through polymerization at the surface of droplets. Both methods produce microcapsules or beads encapsulating ferrous ammonium complexes that are then dried and sieved for analysis.
The document describes two microencapsulation processes: solvent evaporation and surface polymerization. For solvent evaporation, an aqueous solution containing ferrous ammonium sulfate was emulsified in an oil phase containing PMMA and dichloromethane to form microcapsules between 50-500 micrometers. For surface polymerization, an aqueous solution was emulsified in a monomer solution of methyl methacrylate containing an initiator and catalyst to form larger PMMA beads from 250 micrometers to 4 millimeters through polymerization at the surface of droplets. Both methods produce microcapsules or beads encapsulating ferrous ammonium complexes that are then dried and sieved for analysis.
made by dissolving an appropriate After the PVA was dissolved fully, ferrous amount ofPVA 2( inner aqueous phase) ammonium sulfate was dissolved to The oil phase was obtained by dissolving dependent on the required particle size 5% w/w PMMA in dichloromethane make a 0.07M ferrous ammonium (DCM). (2% w/v for 50–100 and 100–250, and solution (as the inner aqueous phase). 6% w/v for 250–500 micrometer) in de- ionized water
To initiate encapsulation, the aqueous with continuous agitation by an RW-16
basic overhead mechanical stirrer at phase was added into the organic speeds ranging from 100 rpm to 600 phase, followed by 2 minutes with Each W/O emulsion was then poured rpm (dependent on the desired particle into 2% w/w PVA solution (outer gentle shaking by hand to make a size; 200 rpm for microcapsules of 250– aqueous phase), Water-in Oil (W/O) emulsion 500 mm; 600 rpm for microcapsules of 50–100 mm) to form the final (5%w/w+DCM)) water/oil/water (W/O/W) emulsions.
After microencapsulation, each mixture
After 30minutes, an additional 100mL was centrifuged at 5000 rpm for 5minutes. All microcapsules were oven dried (60 C) of 0.5% w/w PVA solution was added and weighed before measuring the The microcapsules were then washed percentage encapsulation efficiency to further stabilize and solidify the with de-ionized water three times to microcapsules (%EE). remove the non-encapsulated ferrous ammonium complex and residual PVA
09/02/2020 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 Simultaneously, the 0.07M ferrous The two phases were combined (MMA, liquid) and stirred until ammonium aqueous phase was with gentle agitation using a plastic fully dissolved (as the organic prepared with 6% w/w PVA. rod (1:10, aqueous: organic). phase). .
The catalyst, 0.2mL 4,N,N- A low agitation speed (<150 rpm)
After the beads were formed, the trimethylaniline was then added was maintained to ensure that the whole mixture was agitated at 200 W/O droplets stayed at the surface using a transfer pipette, with of the solution for the rpm for another 30 minutes to continued gentle agitation, to further stabilize and solidify the polymerization procedure to occur PMMA beads. make a W/O emulsion (no higher than 150 rpm).
All PMMA beads were then dried in
The PMMA beads were then an oven overnight at 60 C. Unlike solvent evaporation washed with de-ionized water microencapsulation, a wide range After drying, the PMMA beads were three times to remove the non- (250 mm to 4mm in diameter) of sieved and separated using US encapsulated ferrous PMMA beads can be obtained from standard sieves (three size ranges: a single batch using the surface 0.5–1, 1–2, and 2–3mm) and ammonium complex and polymerization process. weighed before measuring the %EE. residual PVA.