FACULTY OF PHRMACY
TECHNOLOGY PHARMACEUTICAL II
NFNF 2263
LABORATORY
REPORT
PRACTICAL 1: EMULSION
GROUP B4
GROUP B4
LECTURER'S NAME :
DR. NG SHIOW FERN
GROUP MEMBERS:
1. LEE
LI SHAN A136251
2. YIP
LEE ANN A136282
3. MUHAMMAD
SHAHIR BIN ABU BAKAR A136436
4. AINAA
ZURIANI BINTI ABDUL AZIZ A136650
5. NOOR
FARAHIN BINTI ARIFFIN A136602
Practical 1:
Different impact assessment on the content of the
features of an emulsion.
Introduction
Emulsion is a mixture of disperse
system consisting two immiscible liquids where one is dispersed as droplets in
another. The liquid droplets are also known as disperse or internal phase,
while the liquid in which they are dispersed is called continuous or external
phase. The disperse phase or continuous phase of a pharmaceutical emulsion is
usually water and oil. An emulsion is described as oil-in-water (o/w) emulsion
when the continuous phase is water while it may be described as water-in-oil
(w/o) when the continuous phase is oil. Emulsion is highly unstable systems due
to high surface tension that exist between the two phases. Thus, it needs a
third component, which is an emulsifying agent that helps in stabilizing the
emulsion.
Hydrophile-lipophile balance, or HLB
is a method used to determine the quantity and select the appropriate surfactant
that is needed to produce a stable emulsion. It is only applied to non-ionic Tween and Span type emulsifiers. The number 1 to 20 is assigned to each
surfactant to express numerically the size and strength of the polar portion
relative to the non-polar portion of the molecule. The HLB value can be
determined based on the using of this formula:
HLB
value = (quantity surfactant 1)(HLB surfactant 1) +
(quantity surfactant
2)(HLB surfactant 2)
______________________________________
Quantity surfactant 1
+ Quantity surfactant 2
Aim
1-
To
determine the effect of HLB surfactant on the stability of emulsion
2-
To
study the physical and stability effects on the formulation of emulsion due to
the different types of emulsifier agents.
Apparatus
Test tubes, cylinder of 50 ml, two sets of pasture
pipette and droppers, mixing Vortex’s apparatus, weighing boat, mortar and
pestle, light microscope, slides, one set of pipette of 5 ml and bulb, 50 ml
beaker, 15 ml centrifuge, coulter counter apparatus, centrifuge device,
Viscometer device, water bath (45ºC), refrigerator (4ºC).
Materials
Palm oil, arachis oil, olive oil, mineral oil,
distilled water, Span 20, Tween 80, Sudan III solution (0.5ºC), Isoton III solution
Procedure
Every test tube been labeled and 1
cm is drawn from bottom of the test tube. For our group, we mixed 4 ml of
mineral oil and 4 ml of distilled water into the test tube. For every mixing of
oil and water, Span 20 and Tween 80 been dropped. The test tube is closed with
its cap and mixing is done by using Vortex mixing device for 45 seconds. The
time needed for the interphase to reach 1 cm is recorded. The HLB value for
every sample is calculated. Then, a few drops of Sudan III solution are dropped
on 1 gram of emulsion that been produced in a weighing boat and flattened. The
colour distribution of the sample is described and compared. Some of the sample
is taken and flattened on glass slide and observation is done under the light
microscope. The shape and globule size is drawn together with a description and
comparison.
The next experiment is by using wet
gum method, formulation of mineral oil emulsion of 50 g is produced by using
the formula below:
Mineral oil 35 ml
Acacia 6.25 g
Syrup
5 ml
Vanillin 2 g
Alcohol 3 ml
Distilled water, qs 50 ml
All the
substances above are weighed accurately. Based on wet gum method, acacia powder
is added to the mortar and triturated with water until smooth gum is obtained.
Then, oil is added to the mixture while triturating continuously until smooth
emulsion is obtained.
40 g of emulsion that has successful
been produced is put into 50 ml beaker and homogenous process is been conducted
for 2 minute by using magnetic stirrer.
Emulsion
|
Group
|
Mineral oil (ml)
|
I
|
1 , 5
|
20
|
II
|
2 ,6
|
25
|
III
|
3 ,7
|
30
|
IV
|
4 ,8
|
35
|
Table 3
2
g of emulsion that is produced before and after homogenous process is weighed
on weighing boat and been labeled. A few drops of Sudan III solution are
dropped and flattened. The texture, consistency, degree of oil surface and the
spreading of colour are differentiate and describe under light microscope.
The
viscosity of the emulsion that is formed after homogenous process is determined
by using viscometer tool that has been calibrated with ‘Spindle’ from LV-4
type. Later, the sample been exposed at 45 ºC for 30 minutes and 4 ºC for 30
minutes. The viscosity later is determined after the emulsion has completely
exposed under stated temperatures and when the emulsion has reached room
temperature for 10-15 minutes.5 g of emulsion that has been
homogenous is filled in centrifuge tube and centrifugation process is done at
4500 rpm for 10 minutes at 25 ºC. The height separated is measured and the
fraction of the separation that resulted from the emulsion is determined.
Results and Calculation
- The time required to get a separated phase of 1cm.
Palm oil:
Tube No.
|
1
|
2
|
3
|
4
|
5
|
6
|
7
|
8
|
Span 20 (drops)
|
15
|
12
|
12
|
6
|
6
|
3
|
0
|
0
|
Tween 80 (drops)
|
3
|
6
|
9
|
9
|
15
|
18
|
15
|
0
|
HLB value
|
9.67
|
10.73
|
11.34
|
12.44
|
13.17
|
14.09
|
15.00
|
0.00
|
Phase separation time (min)
|
116.00
|
121.00
|
135.00
|
49.00
|
132.00
|
32.00
|
26.00
|
8.00
|
Stability
|
No
|
No
|
No
|
No
|
No
|
No
|
No
|
No
|
Arachis oil:
Tube No.
|
1
|
2
|
3
|
4
|
5
|
6
|
7
|
8
|
Span 20 (drops)
|
15
|
12
|
12
|
6
|
6
|
3
|
0
|
0
|
Tween 80 (drops)
|
3
|
6
|
9
|
9
|
15
|
18
|
15
|
0
|
HLB value
|
9.67
|
10.73
|
11.34
|
12.44
|
13.17
|
14.09
|
15.00
|
0.00
|
Phase separation time (min)
|
-
|
-
|
-
|
45.00
|
37.00
|
18.00
|
77.00
|
2.00
|
Stability
|
Yes
|
Yes
|
Yes
|
No
|
No
|
No
|
No
|
No
|
Olive oil:
Tube No.
|
1
|
2
|
3
|
4
|
5
|
6
|
7
|
8
|
Span 20 (drops)
|
15
|
12
|
12
|
6
|
6
|
3
|
0
|
0
|
Tween 80 (drops)
|
3
|
6
|
9
|
9
|
15
|
18
|
15
|
0
|
HLB value
|
9.67
|
10.73
|
11.34
|
12.44
|
13.17
|
14.09
|
15.00
|
0.00
|
Phase separation time (min)
|
40.00
|
-
|
-
|
64.00
|
59.00
|
21.00
|
34.00
|
5.00
|
Stability
|
No
|
Yes
|
Yes
|
No
|
No
|
No
|
No
|
No
|
Mineral oil:
Tube No.
|
1
|
2
|
3
|
4
|
5
|
6
|
7
|
8
|
Span 20 (drops)
|
15
|
12
|
12
|
6
|
6
|
3
|
0
|
0
|
Tween 80 (drops)
|
3
|
6
|
9
|
9
|
15
|
18
|
15
|
0
|
HLB value
|
9.67
|
10.73
|
11.34
|
12.44
|
13.17
|
14.09
|
15.00
|
0.00
|
Phase separation time (min)
|
-
|
-
|
-
|
-
|
55.00
|
47.00
|
12.00
|
0.00
|
Stability
|
Yes
|
Yes
|
Yes
|
Yes
|
No
|
No
|
No
|
No
|
Test Tube
|
Physical Characteristics
|
1
|
Naked eye:
·
Sudan III not soluble
Microscopic:
·
Small globules evenly dispersed
·
Globules stained red
Thus, it is
oil in water emulsion
|
2
|
Naked eye:
·
Sudan III not soluble
Microscopic:
·
Small globules evenly dispersed
·
Globules stained red
Thus, it is
oil in water emulsion
|
3
|
Naked eye:
·
Sudan III not soluble
Microscopic:
·
Small and large globules dispersed
·
Globules stained red
Thus, it is
oil in water emulsion
|
4
|
Naked eye:
·
Sudan III not soluble
Microscopic:
·
Small and large globules dispersed
·
Globules stained red
Thus, it is
oil in water emulsion
|
5
|
Naked eye:
·
Sudan III not soluble
Microscopic:
·
Small and large globules dispersed
·
Globules stained red
Thus, it is
oil in water emulsion
|
6
|
Naked eye:
·
Sudan III not soluble
Microscopic:
·
Small and large globules dispersed
·
Globules stained red
Thus, it is
oil in water emulsion
|
7
|
Naked eye:
·
Sudan III not soluble
Microscopic:
·
Small and large globules unevenly dispersed
·
Globules stained red
Thus, it is
oil in water emulsion
|
8
|
Naked eye:
·
Sudan III not soluble
Microscopic:
·
Small and large globules very unevenly dispersed
·
Globules stained red
Emulsion is
not formed without surfactant, phase separation occur very fast
|
Emulsion
|
Characteristics
|
I
|
Before homogenization
·
Naked eyes: less milky, less viscous, more oily
·
Microscopic: more
globules, red stain is unevenly dispersed
After homogenization
·
Naked eyes: milky, more viscous, less oily
·
Microscopic: less and smaller globules, red stain evenly dispersed
|
II
|
Before homogenization
·
Naked eyes: milky, oily, less viscous
·
Microscopic: many globules, red stain is unevenly dispersed
After homogenization
·
Naked eyes: more viscous, less oily
·
Microscopic: less and smaller globules, red stain evenly dispersed
|
III
|
Before homogenization
·
Naked eyes: cloudy, less viscous, more oily
·
Microscopic: more globules, red stain is unevenly dispersed
After homogenization
·
Naked eyes: milky, more viscous, less oily
·
Microscopic: smaller globules, red stain evenly dispersed
|
IV
|
Before homogenization
·
Naked eyes: cloudy, less viscous, more oily
·
Microscopic: not uniform in size, red stain is unevenly dispersed
After homogenization
·
Naked eyes: milky, more viscous, less oily
·
Microscopic: smaller globules , uniform in size, red stain evenly
dispersed
|
3. VISCOSITY OF EMULSION :
Difference = Average
of after temperature cycle-
Average of before temperature cycle x 100%
Average
of before temperature cycle
At 20 mL of Palm Oil:
Readings
|
Group
|
Viscosity (cP)
|
Average + SD
|
||
1
|
2
|
3
|
|||
Before
temperature cycle
|
1
|
150
|
100
|
150
|
78.33 ± 57.57
|
5
|
20
|
20
|
30
|
||
After temperature
cycle
|
1
|
200
|
200
|
250
|
114.17 ±
103.86
|
5
|
10
|
10
|
15
|
||
Difference (%)
|
45.76%
|
||||
At 25 mL of Arachis Oil:
Readings
|
Group
|
Viscosity (cP)
|
Average + SD
|
||
1
|
2
|
3
|
|||
Before
temperature cycle
|
2
|
30
|
60
|
120
|
60.00 ± 28.28
|
6
|
50
|
50
|
50
|
||
After
temperature cycle
|
2
|
120
|
120
|
90
|
105.00 ± 11.18
|
6
|
100
|
100
|
100
|
||
Difference (%)
|
75%
|
||||
At 30 mL of Olive Oil:
Readings
|
Group
|
Viscosity (cP)
|
Average + SD
|
|||
1
|
2
|
3
|
||||
Before
temperature cycle
|
3
|
420
|
480
|
540
|
490.00 ± 46.19
|
|
7
|
450
|
500
|
550
|
|||
After
temperature cycle
|
3
|
2800
|
2650
|
2460
|
2626.67 ±
219.97
|
|
7
|
3000
|
2500
|
2350
|
|||
Difference (%)
|
436.06%
|
|||||
For 35 mL of Mineral Oil :
Readings
|
Group
|
Viscosity (cP)
|
Average + SD
|
||
1
|
2
|
3
|
|||
Before
temperature cycle
|
4
|
5750
|
5800
|
5850
|
7363.33 ±
1563.83
|
8
|
8900
|
8900
|
8980
|
||
After
temperature cycle
|
4
|
7300
|
7100
|
7200
|
11325.00 ±
4129.14
|
8
|
15650
|
15600
|
15100
|
||
Difference (%)
|
53.80%
|
||||
SEPARATION HEIGHT
Height ratio = Separation phase
Emulsion
phase
20
mL Coconut Oil :
Interphase
|
Height
(mm)
|
Average
|
|
Group
1
|
Group
5
|
||
Separation phase
|
29
|
40
|
|
Original emulsion
|
46
|
50
|
|
Height ratio
|
0.63
|
0.80
|
0.715
|
25 mL Arachis Oil :
Interphase
|
Height
(mm)
|
Average
|
|
Group
2
|
Group
6
|
||
Separation phase
|
33
|
35
|
|
Emulsion phase
|
55
|
50
|
|
Height ratio
|
0.64
|
0.70
|
0.670
|
30
mL Olive Oil :
Interphase
|
Height
(mm)
|
Average
|
|
Group
3
|
Group
7
|
||
Separation phase
|
14
|
11
|
|
Emulsion phase
|
50
|
50
|
|
Height ratio
|
0.28
|
0.22
|
0.250
|
35 mL Mineral Oil :
Interphase
|
Height (mm)
|
Average
|
|
Group 4
|
Group 8
|
||
Separation phase
|
15
|
11
|
|
Emulsion phase
|
55
|
50
|
|
Height ratio
|
0.27
|
0.22
|
0.245
|
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