Department of Pharmacy MIPT645 Experiment #5 Suspensions: Name

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Department of Pharmacy

MIPT645
Experiment #5

“Suspensions”

Name: Tujan Liddawieh


Mayson Bali

Instructor: Dr. Moammal Qurt


(2019, 1st semester)
Suspensions
Suspensions are a class of dispersed system in which a finely divided solid is dispersed
uniformly in a liquid dispersion medium, classified as coarse or colloidal dispersion, depending
on the size of particles. Typically, the suspensions with particle size greater than 1µm are
classified as coarse suspension, while those below 1µm are classified as colloidal suspension.
When the particles constituting the internal phase of the suspension are therapeutically active, the
suspension is known as pharmaceutical suspension. Depending on their intended route of
delivery, pharmaceutical suspensions can be broadly classified as parenteral suspension, topical
suspensions, and oral suspensions.

Experiment 1: Simple Syrup (BP)

Aim: To prepare and dispense simple syrup.

Requirements: Sucrose, beaker, stirrer, spatula, measuring cylinder and purified water.

Principle: Syrups are sweetened, viscous, concentrated solutions of sucrose or, other sugars in
water or any other suitable aqueous vehicles. These are further classified into two classes.

1. Simple flavor syrups: Do not contain any medicament or drug. These syrups are used as a
vehicle for other Liquid preparation to mask the disagreeable taste of drug.
2. Medicated syrups: These contain some medicinal substance along with their other
additives. Sucrose concentration in simple syrup is a 66.7%w/w.

Procedure
1- Add approx. 110 ml water to glass beaker.
2- Heat while mixing using magnetic stirrer.
3- Add Sucrose gradually while mixing.
4- Adjust volume to 250 ml using purified water while mixing until completely dissolved.

Sedimentation volume

Sedimentation means settling of particle (or) floccules occur under gravitational force in liquid
dosage form.

Sedimentation Parameters

- Sedimentation volume (F) or height (H) for flocculated suspensions.


- Definition: Sedimentation volume is a ratio of the ultimate volume of sediment (Vu) to
the original volume of sediment (VO) before settling.
- F = V u / VO Where, Vu = final or ultimate volume of sediment, VO = original volume
of suspension before settling.
F has values ranging from less than one to greater than one. When F < 1 which mean Vu < Vo or
When F =1 which mean Vu = Vo The system is in flocculated equilibrium and show no clear
supernatant on standing. When F > 1 which mean Vu > Vo Sediment volume is greater than the
original volume due to the network of floccules formed in the suspension and so loose and fluffy
sediment. The sedimentation volume gives only a qualitative account of flocculation.

Experiment 2: Zinc oxide suspension

Materials Weight Function Melting Solubility


range
Zinc oxide 5%(5g) Skin protective from 1,974C˚ It is nearly insoluble in water,
irritation. Widely (decomposes) but it will dissolve in
used to treat a most acids, such
variety of skin as hydrochloric acid. Solid
conditions, including zinc oxide will also dissolve in
dermatitis, itching alkalis to give soluble zincates
due to eczema,
diaper rash and acne.
It was formerly used
as an orally
administered
medicine for
epilepsy, and later
for diarrhea.

Syrup up to Vehicle, sweetening


100% agent, preservative.
Table 1. Materials properties

Procedure

1- Triturate zinc oxide with a small quantity of syrup in a mortar.


2- Add slowly small amounts of syrup while
triturating.
3- Continue until all the syrup is added.
4- Transfer to a graduated Cylinder and cover
with a para film.
5- Leave the suspension for sedimentation.
Questions

1- Calculate the sedimentation volume F


Sedimentation volume is a ratio of the ultimate volume of sediment (Vu) to the original
volume of sediment (VO) before settling.
F = V u / VO Where, Vu = final or ultimate volume of sediment, VO = original volume
of suspension before settling.
Formula No1. Zinc oxide suspension
VO =100, Vu= 10
10÷100*100% = 0.1 which mean 10% volume of the suspension is occupied by the loose
flocs as the sediment.
Formula No2. Chloramphenicol suspension
Vo = 100, Vu = 49
49÷100*100% = 0.49 which mean 49% volume of the suspension is occupied by the
loose flocs as the sediment.

2- How can you increase the stability of this suspension


1- Ensure That Particles Remain Discrete and Uniformly Suspended:
A number of factors contribute to the maintenance of particles in a stably dispersed state,
and these may be classified as either kinetic or thermodynamic in origin.
 Kinetic stability is facilitated by:
Slowing down Brownian motion, inhibiting aggregation and decreasing sedimentation. 
 Thermodynamic stability is facilitated by:
Changing the size or shape of a particle or the electrostatic charge it carries.
2- Promote the formation of loose flocculants that are easily redispersed with shaking.
3- Induce a network gel in the continuous phase:
An alternative way of inducing stability in suspensions where gravitational forces
dominate is to introduce a network structure into the continuous phase to give the system
a yield stress. Systems with a yield stress remain stationary and do not flow until the
applied shear exceeds a certain value. Such suspensions therefore exhibit kinetic stability
with particles remaining stationary and suspended within the network, if any applied
stress does not exceed the yield stress.
4- Promoting a number of physical and chemical properties of the suspension, including
particle size, rheology and zeta potential.
Particle size:
 In a submicron suspension, Brownian motion helps to keep the particles in a dispersed
state.
 For larger particles, the effect of gravity becomes significant, especially if there is a
sizeable difference in density between the dispersed and continuous phases.
 The ratio of gravitational to Brownian forces therefore correlates with the likelihood of
sedimentation.
 According to Stokes’ law, the velocity of a suspended particle falling under gravity is
directly proportional to the particle’s size. Reducing the size of suspended drug particles
therefore reduces the rate and likelihood of sedimentation, helping to maintain the
dispersion. However, if particles still settle although they are fine, the result may be rigid
aggregates and a compact cake that resists breakup and is not easily dispersed.
Rheology:
 For a dilute suspension, Stokes’ law states that the sedimentation velocity is inversely
proportional to the viscosity of the continuous phase, as well as being proportional to
particle size. For particles of a given size, doubling the suspension viscosity will
therefore halve the rate of sedimentation. However, settling behavior is more complex in
more concentrated suspensions, due to interactions between neighboring particles and the
fact that high particle loading leads to an increase in overall density and viscosity.
Zeta Potential:
 Zeta potential provides a measure of the magnitude of the electrostatic or charge
repulsion/attraction between particles at the slipping plane, between the particle and its
associated double layer, and the surrounding solvent.
 If a suspension has a large negative or positive zeta potential, the particles within it tend
to successfully repel each other, whereas smaller negative or positive zeta potential
values increase the flocculation. The dividing line between stable and unstable
suspensions is generally taken as ±30 mV, with systems with zeta potentials which are
respectively more positive or negative than this conferring suspension stability.
3- Is this system Flocculated or deflocculated and why
 The value of a deflocculated suspension is relatively small, 0.2.
 Suspension with F value 1 is the ideal system
 This system is deflocculated, F value is 0.1 and 0.49

Experiment 3: Chloramphenicol suspension


Materials Weight Function Melting Solubility
range
Chloramph 4g API, Antibacterial 90C˚ Chloramphenicol Palmitate is
enicol (systemic- can cause soluble in ethanol, methanol, DMF
palmitate hematologic toxicity) and DMSO.

Glycerin 20g Antimicrobial preservative; 17.8C˚ In acetone Slightly soluble in


cosolvent; emollient; Benzene Practically insoluble in
humectant; plasticizer; Chloroform Practically insoluble in
solvent; sweetening agent; Ethanol in Oils Practically
tonicity agent. insoluble and Water Soluble

Xanthan 0.2g Gelling agent; stabilizing 270C˚ Practically insoluble in ethanol and
gum agent; suspending agent; ether soluble in cold or warm water.
sustained-release agent;
viscosity-increasing agent

Flavoring q.s Masking the drug . Flavoring agents are often thermo
agent unpleasant taste, coating labile and so cannot be added prior
drug particles to an operation involving heat. The
flavor and color should also
complement each other
Simple 50g Vehicle, sweetening agent,
syrup preservative.
Water Up to Vehicle and solvent. 0C˚ Miscible with most polar solvents.
100ml
Table 2. Materials properties

Procedure
1. Triturate Chloramphenicol palmitate with Glycerin and xanthan gum in a
mortar to give a smooth pourable paste.
2. Dilute the paste with simple syrup , mix.
3. Transfer to a beaker , then add the rest of the syrup and add the flavor.
4. Complete to volume with water.
5. Transfer to a clean bottle and fix a label.

Questions
1- How can you modify the system flocculation
Controlled flocculation can be achieved by a combination of control of particle size
and the use of flocculating agents.
Flocculating agents examples:
Electrolytes: act by reducing the zeta potential, which brings the particles together to
form loosely arranged structures. The flocculating power increases with the valency of
the ions.
Polymers: Linear and branched chain polymer form a gel-like network that adsorbs
onto the surface of dispersed particles, holding them in a flocculated state. Moreover,
hydrophilic polymers can also function as protective colloids.
Surfactants: for example nonionic surfactants. Forming particles collide, loosely
packed aggregates of particles or flocs are created

Experiment 4: Ranitidine suspension

Prepare 50 ml of suspensions containing 1%(W/V) ranitidine hydrochloride from


available tablet which contains 150 mg ranitidine hydrochloride per tablet . The
suspension also contains 50%(V/V) sugar syrup, 0.9% (W/V) Xanthan gum and
Purified water .

Ingredient Percentage Quantity


Ranitidine 1% (500mg, 1000mg of
hydrochloride ranitidine tablet, wt.
of 4 tablets)
Xanthan gum 0.9% (0.45 g)
Sugar syrup 50% (25ml)
Purified water Up to 100ml Up to 100ml (55 ml)

Ranitidine hydrochloride (API):


 Is a member of the class of histamine H2-receptor antagonists with
antacid activity.
 soluble in water
 melting range 96-70C˚
Procedure
1- Calculate the quantity of each ingredient for the amount to be prepared.
2- Accurately weigh or measure each ingredient.
3- Grind five tablets of ranitidine tablets using a mortar and pestle until fine
powders are formed.
4- Weigh 500 mg of the ranitidine powder.
5- Mix the ranitidine powder with a small quantity of syrup, geometrically, add
25ml of syrup to form a smooth paste.
6- Geometrically, add Purified water to final volume and mix well.
7- Package and label.

Calculations: for preparing 50ml of suspension.


Ranitidine: 1% w/v, 1g/50ml *100ml=0.5g (500mg) Wt. Of API
Each tablet contain 150mg of API with tablet weight of 300mg (300/500*150 =
1000mg Wt. of tablets needed so 1000/300 = 3.3 No. of tablets needed).
Sugar syrup: 50% v/v, 50ml/50ml*100ml =25ml of syrup needed.
Xanthan gum: 0.9% w/v, 0.9g/50ml*1ooml=0.45g needed.
Experiment 5: Viscosity & Rheology

Prepare the following gel w/w:


Ingredients
Xanthan gum 1%
Water up to 300g

Procedure
Add xanthan gum to water and mix vigorously until clear
Use homogenizer mixer for mixing
Using Brookfield viscometer determine the rheological behaviour of the gel.

Questions

1. State the function of each ingredient


Xanathan gum is a gelling agent; stabilizing agent; suspending agent; sustained-release
agent; viscosity-increasing agent.

2. Suggest an experiment to flocculate the suspension


Flocculation is obtained by adding a flocculation agent like surfactant or a polymer in a
sufficient amount.
Experiment example:
 Triturate zinc oxide with a small quantity of syrup in a mortar
 Add slowly small amounts of syrup while triturating
 Continue until all the syrup is added.
 Make three samples one without surfactant one with SLS and the last with
tween 80
 Transfer each sample to a graduated Cylinder and cover with a para film
 Leave the suspension for sedimentation

3. What type of Rheological behavior the xanthan gum gel have?


The rheological behavior of xanthan gum in aqueous solutions at room temperature
indicates a shear-thinning behavior related to the orientation of molecules along the
flow. At low shear rates, the stretching polysaccharide molecules intertwine
to form aggregates that cause high viscosity

4. What factors affect the Viscosity measurements


 Temperature: as temperature increase viscosity will decrease.
 Pressure: there are two types of materials that could be affected differently by
pressure. The first type the Newtonian in which as the pressure and the
viscosity is direct relation as the pressure increases the viscosity increase and
vice versa.The other type is the non-Newtonian in which when the pressure
increase the viscosity will decrease, this is called shear thinning.
 Amount and type of thickening agent.

5. How can we measure the degree of flocculation for a suspension


To determine the degree of flocculation, flocculated suspensions were made using
flocculation agent. The sedimentation volume were determined by keeping specific
amount of each suspensions in measuring cylinder and stored undisturbed at room
temperature then comparing the amount sediment to the total volume.

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