4. 10/20% (w/v) CM-TG: Weigh 10/20 g of CM-TG of DS 1.2
into a volumetric flask (100 mL) and add distilled water up to
the graduated mark. Stir the mixture at 600 rpm for 10 min
using an automated stirrer. Adjust the pH of the mixture to
4 using glacial acetic acid.
3 Methods
3.1 Aluminium
and Irradiation
Cross-linked Beads by
Conventional
Ionotropic Gelation
1. Incorporate 5-ASA into 50 mL of 10% CMSP solution by
adding 10, 20, and 30% (w/w) of 5-ASA of total CMSP used
directly and using automated magnetic stirrer for 15 min at
800 rpm (see Note 3). Add 0.1% (w/w) of sodium metabisulfite, sonicate at 80% amplitude for 2 min [7].
2. Use the conventional ionotropic method by dripping the
10 mL of CMSP/5-ASA solution into a stirring 5% (w/v)
aluminum chloride (AlCl 3 ) solution (see Note 4) that contains
0.1% (w/w) sodium metabisulfite using a 10 mL syringe with
18-gauge needle tip at a distance of 6 cm from the cross-linking
solution (see Note 5) within a 2 min introduction time span to
form the beads. Leave the beads to cure for 15 min, then collect
and dry them at 40
C for 24 h to constant weight. Store the
beads at 10
C.
3. For further cross-linking, subject freshly prepared CMSP/5ASA beads to electron beam irradiation at 10 kGy (see Notes 6
and 7). Then, dry the beads at 40
C for 24 h to constant
weight. Store the beads at 10
C.
3.2 Calcium
and Irradiation
Cross-Linked Beads by
Conventional
Ionotropic Gelation
1. Dissolve 10% (w/w) of diclofenac sodium based on the CMSP
and pectin total weight in distilled water. Dissolve 15%/5%
(w/v) CMSP/pectin in the same solution stir for 30 min at
600 rpm using automated magnetic stirrer followed by
homogenization (see Note 8) [10].
2. Use the conventional ionotropic gelation method within a
2 min introduction time span to form the beads by manually
dripping 10 mL of CMSP/pectin/diclofenac solution into a
magnetically stirring 10% (w/v) calcium chloride solution at
pH 3.6 (see Note 9). Use a 10 mL syringe with a 21-gauge
hypodermic needle tip at a distance of 6 cm from the crosslinking solution (see Note 5). Leave the beads to cure for
20 min. Remove the beads via filtration and wash using distilled
water.
3. For further cross-linking, subject the beads to electron beam
irradiation at 5, 10, 15, and 20 kGy (see Note 10). Dry at 37
C
for 24 h to obtain constant weight.
176
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