PHARMACEUTICS-VIA

(PHARMACEUTICAL QUALITY
MANAGEMENT) [THEORY] PHARM 618
Department of Pharmaceutics ,Faculty of Pharmacy ,University of Sindh Jamshoro
QUALITY CONTROL OF
DISPERESE SYSTEMS
Tests for Emulsions and Suspension
 TEST FOR EMULSION
• The type of Emulsion

• pH

• Water content of Emulsions

• Dispersibility

• Physical stability of Emulsions

• Content Uniformity and Assay for Active Ingredient

 TEST FOR EMULSION
• The type of Emulsion
• Color test
• Physical Test
• Dilution test
• Filter paper wetting test
• Dye test
• Conductivity test
 TEST FOR EMULSION
• pH:
• pH can affect the stability of active ingredients and physiological
suitability.
• Therefore maintenance of specific pH value is mandatory for
optimum stability.
• In emulsions an important parameter that determine pH is
emulsifier system.
 TEST FOR EMULSION
• pH;
• Emulsions based on soaps usually have a pH of 8 or more.
• Emulsions having a pH greater than 9 do not contain esters because
of saponification.
• Those at pH less than 7 can be emulsified with non-ionic,cationic or
acid stable anionic substances.
• pH meter(glass electrode equipment) or test papers
 TEST FOR EMULSION

Water content of Emulsions;

• One of the best method for water content determination is
Karl Fischer titration.
• If the emulsion is alkaline ,a correction may usually be
made for the water produced by the reaction of free alkali
and acid from titration reactants.
 TEST FOR EMULSION
Dispersibility:
• Dispersibility of emulsion is determined by the continuous phase.
• Thus if the continuous phase is water-soluble, the emulsion may be diluted with
water
• Conversely , if the continuous phase is oil-soluble, the emulsion may be diluted
with oil.
• The effects of Dispersibility on skin are considerably important.
• Unique properties are often observed if a formula is designed to combine
unusual application effects and thus may be on borderline of Dispersibility and
type of emulsion.
 TEST FOR EMULSION
Physical stability of Emulsion:
• Stability of a Pharmaceutical emulsion is characterized by the
absence of coalescence of the internal phase(dispersed phase
globules merge together and for big globules), creaming(Rise of
dispersed particles to the emulsion surface)
• Maintenance of elegance with respect to appearance, odor, color etc.
• In Pharmaceutical emulsion creaming can result in lack of
uniformity of drug distribution and possibly to a variable dosage.
 TEST FOR SUSPENSIONS
• pH
• Particle size distribution
• Sedimentation volume of Suspension
• Crystal Growth in Suspension
• Surface tension
• Viscosity
• Assay and Content Uniformity test for Sterile Suspensions
 TEST FOR SUSPENSIONS
pH:
• For the determination of pH in suspensions it is suggested that
suspension to be centrifuged prior to the test,
• Otherwise results may differ by up to three pH units.
• pH meter or litmus paper is used for determination.
 TEST FOR SUSPENSIONS
Particle Size Distribution
• A general range is between 1-50 micrometer.
• The particle size distribution is performed by using a microscope.
• Mix equal volume of sample and glycerin/liquid paraffin(as
specified in monograph),further can be diluted with glycerin and
water(mixture in equal volumes) if needed.
• Mount the dilute preparation on slide and analyze the particles.
• Count the number of particle having maximum diameters above or
below the limiting sizes permitted in individual monograph.
 TEST FOR SUSPENSIONS
Particle Size Distribution
• The percentage is calculated from observations on at least 1000
particles.
• Particle size > 5micron cause grittiness and cause irritation in eyes
etc
• Too small particle size tend to form a hard cake at the bottom of
container
 TEST FOR SUSPENSIONS
Sedimentation Volume
• Volume of sedimentation can determine the pharmaceutical
acceptability of suspension.
• The sedimentation volume, F is defined as the ratio of the final or
ultimate volume of the sediment Vu to the original volume of the
suspension VO.
• Formula
• F= Vu / VO
 TEST FOR SUSPENSIONS
Sedimentation Volume
• Suspension formulation(50ml) is poured separately into 100ml
measuring cylinders (at least 3) and sedimentation volume is read
after 1,2,3 and 7 days and then at weekly intervals for 12 weeks.
• Calculate sedimentation volume with the help of formula. The
values ranges 0-1 ,can be greater than 1
• F< 1=> Vu < VO
• F>1=> Vu >VO, because of loose and fluffy sediment
• F= 1=> Vu = VO ,then the product is said to be flocculation
equilibrium and are pharmaceutically acceptable.
 TEST FOR SUSPENSIONS
Crystal Growth in Suspension
• It is also known as Ostwald ripening.
• It is also a cause of deterioration in suspensions due to temperature
fluctuations under normal storage conditions.
• The test is performed by acceleration of crystal growth in
suspensions by stimulation of temperature fluctuations between 23 0
and 330 using a cycling time of 16 minutes.
 TEST FOR SUSPENSIONS
Surface Tension/Interfacial Tension
Two methods
Wilhelmy plate method
• Principle: The force necessary to detach a plate from the surface or
interface of two immiscible liquids is proportional to the surface or
interfacial tension, respectively.
Ring detachment/ du Nouy’s ring Method
• The du Nouy’s ring method uses a ring or loop of wire( platinum or
Iridium wire of ~4 cm in circumference)
• Measured in milli-newtons per meter (mN/m)
 TEST FOR SUSPENSIONS
Viscosity
• Viscosity of suspension depends upon concentration of thickening
agent.
• Determined by using viscometers.
 TEST FOR SUSPENSIONS
Assay and Content Uniformity Test for Sterile Suspensions/Emulsions
• Assay 10 units individually, unless otherwise specified in the
Procedure for content uniformity”
• The requirement meet if the result obtained from each 10 containers
fall within the limits of 85-115% of the average limits specified.
• If not more than 1 result falls outside 85-115% and within 75-125%
of that average value of 20 more containers individually.
REFERENCES

 The Theory & Practice of Industrial Pharmacy, Lachman & Lieberman, pp:672-676.
 Remington, vol.1 Theory and practice of industrial pharmacy
 Quality Management by Kramat A Javed
THANK YOU