pH-SENSITIVE BIO-POLYMER (PHARMACIAL WASTE) WAS PREPARED BY

IONOTROPIC GELATION WITH POTENTIAL APPLICATION TO RELEASE

OF 5-FLUOROURACIL TO COLON
Instructor: Ph.D Tran Hoai Khang
Writer by Tien Ngo
Team: Tien Ngo (leader)
Hong Ha
Phuc Vinh

I. DETERMINATION OF THE OPTIMAL WEIGHT PERCENT OF

k-CARRAGEENAN:
What is k-Carrageenan (k-CG)?
Which k-CG was crosslinked to?
What is Xanthan gum (XG)?
1. THE BEST WEIGHT PERCENT:
k-CG a (7, 8, 9, 10, 11, 12, 13, 14) wt. % solution was prepared in distilled water
with continuous stirring at 80 oC, at 1h. After that, k-CG a wt. % solution (70 oC) added
drop-wise into KCl solution which was submerged in cryogen (0 oC). Then, k-CG a wt. %
beads were immersed about 30 mins, washed with distilled water. Finally, k-CG a wt. %
beads were dried at 80 oC, approximately 5h.
Dried k-CG a wt. % beads were weight minium (0.1 g) and allowed swelling at 37
o
C in pH=7.4 (PBS) in (0.5h, 1h, 2h, 3h,…). The swelling degree was calculated as the
formular below:
W s−W d
Swelling degree ( % )= ×100 %
Wd

Where Ws (g) is the weight of swollen beads at time t, Wd (g) is the initial weight
of the beads.
Parallelly, swelling experiments had to be tested by 4 samples, the experimental
data obtained are expressed as the mean + standard deviation (mean + SD) with statistical
significance defined ass a p-value<0.05.
Sample k-CG (wt. %) KCl (M) Time crosslinking
 (min)
K-01 7 1 30
K-02 8 1 30
K-03 9 1 30
K-04 10 1 30
K-05 11 1 30
K-06 12 1 30
K-07 13 1 30
K-08 14 1 30

1.1. K-01:

Picture 1.1: a) k-CG 7 wt. % beads before drying. b) k-CG 7 wt. % beads after drying.

1.2. K-02:

Picture 1.2: a) k-CG 8 wt. % beads before drying. b) k-CG 8 wt. % beads after drying.

1.3. K-03:
Picture 1.3: a) k-CG 9 wt. % beads before drying. b) k-CG 9 wt. % beads after drying.
1.4. K-04:

Picture 1.4: a) k-CG 10 wt. % beads before drying. b) k-CG 10 wt. % beads after
drying.
1.5. K-05:
Picture 1.5: a) k-CG 11 wt. % beads before drying. b) k-CG 11 wt. % beads after drying.

1.6. K-06:
Picture 1.6: a) k-CG 12 wt. % beads before drying. b) k-CG 12 wt. % beads after
drying.
1.7. K-07:
 Picture 1.7: a) k-CG 13 wt. % beads before drying. b) k-CG 13 wt. % beads after
drying.

1.8. K-08:
Picture 1.8: a) k-CG 14 wt. % beads before drying. b) k-CG 14 wt. % beads after
drying.
1.9. Overall:

2. THE BEST OF MOLARITY KCl: (time crosslinking at 30 min)

k-CG a wt. % was crosslinked in KCl a (0.5, 0.75, 1.0, 1.25) M at 30 mins. After
that, k-CG a wt.% was washed with distilled water and dried at 80 oC, about 3h. At the
end, the swelling degree of k-CG 9 wt. % beads were studied at 37 oC, in pH=7.4.
Time crosslinking
Sample k-CG (wt. %) KCl (M)
(min)
KKC-01 0.5 30
KKC-02 0.75 30
KKC-03 1 30
KKC-04 1.25 30

2.1. KKC-01:
Picture

2.2. KKC-02:
Picture
 2.3. KKC-03:
Picture:

2.4. KKC-04:
Picture
2.5. Overall:

3. DETERMINATION OF THE BEST TIME FOR CROSSLINKING:

k-CG a wt. % was crosslinked in KCl 1 M at a (15, 30, 60) mins. After that, k-CG a wt.%
was washed with distilled water and dried at 80 oC, about 3h. At the end, the swelling
degree of k-CG a wt. % beads were studied at 37 oC, in pH=7.4.
Time crosslinking
Sample k-CG (wt. %) KCl (M)
(min)
KT-01 1 15
KT-02 1 30
KT-03 1 60

3.1. KT-01:
Picture

3.2. KT-02:
Picture

3.3. KT-03:
Picture
3.4. Overall:
4. THE RATIO OF k-CARRAGEENAN/XANTHAN GUM:
k-CG/XG solution was prepared in distilled water with continuous stirring at 70
o
C, at 1h. The ratio of k-CG/XG is 100:00, 99:01, 98:02, 97:03, 96:04, 95:05 w/w. k-
CG/XG solution was added drop-wise into KCl M, which was submerged in cryogen.
Then, k-CG/XG beads were immersed about 30 mins, washed with distilled water.
Finally, k-CG a wt. % beads were dried at 80 oC, approximately 3h.
Dried k-CG a wt. % beads were weight minium (0.01 g) and allowed swelling at
o
37 C in pH=7.4 in 8h (0.5h, 1h, 2h, 3h, 4h, 5h, 6h, 7h, 8h).
Bio-polymer k-CG/XG Time crosslinking
Sample KCl (M)
(wt. %) (w/w) (min)
KXG-01 99:01 30
KXG-02 98:02 30
KXG-03 97:03 30
KXG-04 96:04 30
KXG-05 95:05 30

4.1. 99:01:
Picture

4.2. 98:02:
Picture

4.3. 97:03:
Picture
4.4. 96:04:
Picture
4.5. 95:05:
Picture
4.6. Overall:
5. THE SWELLING DEGREE:
The swelling degress was studied in pH=a (1.2, 6.8, 7.4), which were prepared
from solution Hydrochloride acid, Potassium chloride, PBS, t=37 oC.
5.1. pH=1.2:
5.2. pH=6.8:
5.3. pH=7.4:
 5.4. Overall:
II. DETERMINATION OF THE BEST WEIGHT PERCENT OF
ZEIN (layer 1):
1. THE BEST WEIGHT PERCENT:
1.1. 15 wt. %:
1.2. 20 wt. %:
1.3. 25 wt. %:
1.4. 30 wt. %:
1.5. 35 wt. %:
1.6. 40 wt. %:
2. THE SWELLING DEGREE:
2.1. pH=1.2:
2.2. pH=6.8:
2.3. pH=7.4:
III. THE RELEASE 5-FU:
1. DETERMINE THE OPTIMAL WEIGHT OF 5-FLUOROURACIL WERE
ENCAPSULATED BY …:
W1
Drug loading efficiency (¿) ( % )= ×100 %
W0
W1: The amount of 5-FU in microbeads. (g)
W0: the amount of 5-FU added during loading process (0.5g drug was used in
this experiment). (g)
W1
Drug loading content (LC) ( % )= ×100 %
W2
W2: The amount of weight microbeads. (g)
Drug delivery system in 8 hours, with 2h in pH 1.2, 3h in pH 6.8, 3h in pH 7.4.
1.1. CORE: (CACULATE 3 FORMULAR)
1.2. CORE-SHELL: (CACULATE 3 FORMULAR)
2. BIODEGRADATION:
IV. THERMALGAVIMATRIC ANALYSE (TGA):
V. FTIR:
VI. SEM: