This presentation is knowledge about the in process and finished product quality control test for semi solid dosage form e.g. Cream , ointment , suppository , gel etc. And procedure for the perform test for semi solid dosage form.

1. Presented by : Mansi Vadodariya
M.Pharm
Semester 1
IPQC and FPQC Tests for
Semi Solid Dosage Form
DEPARTMENT OF PHARMACEUTICAL QUALITY ASSURANCE
L.M. COLLEGE OF PHARMACY

2. CONTENTS
 Introduction
 Ideal properties
 Categories of semi solid dosage form
 What is IPQC ?
 What is FPQC ?
 Quality Control Test for Topical Dosage
Form
 Evaluation of Gels
 Evaluation of Suppositories
 References

3.  Semisolid pharmaceutical systems comprise a body of products,
which when applied to the skin or accessible mucous membranes
tend to treat a pathological condition or offer protection against a
harmful environment.
 They have the property to cling to the skin or mucous membrane for
a protracted period of time to exert their therapeutic effect through
protection.
 DEFINITION: Semisolid dosage forms are dermatological products
of semisolid consistency which are applied to skin or mucous
membrane for therapeutic or protective action or cosmetic function.
INTRODUCTION

4.  They can be applied topically to the skin, cornea, rectal tissue, nasal
mucosa, vagina, buccal tissue, urethral membrane, and external ear
lining.
 Ointments, creams, pastes and gels are semisolid dosage form intended
for topical application.

5.  PHYSICAL PROPERTIES
 Smooth texture
 Elegant in appearance
 Non dehydrating
 Non gritty
 Non greasy and non staining
 Non hygroscopic
IDEAL PROPERTIES

6.  PHYSIOLOGICAL PROPERTIES
 Non irritating
 Do not alter membrane / skin functioning
 Miscible with skin secretion
 Have low sensitization index
 APPLICATION PROPERTIES
 Easily applicable with efficient drug release.
 High aqueous wash ability.

7. CATEGORIES OF SEMI SOLID DOSAGE FORM
Semi Solid Dosage Form
INTERNAL
Suppositories
Pessaries
EXTERNAL
Ointments
Creams
Pastes
Jellies / Gels
Poultices
Plasters
Glycero-gelatins
Rigid forms

8. OINTMENTS
• Ointments are semisolid preparations meant for external application to the
skin or mucous membrane. They usually contain a medicament or
medicaments dissolves, suspended or emulsified in the base.
CREAMS
• Creams are viscous emulsions of semisolid consistency intended for
application to the skin or mucous membrane.
1. O /W type
2. W/O type
PASTES
• Pastes are the preparations contain a large amount of finely powdered solids
such as starch and zinc oxide. These are generally very thick and stiff.

9.  JELLIES
• These are thin transparent or translucent, non greasy preparations.
They are similar to mucilages because they are prepared by using gums
but they differ from mucilages in having gelly like consistency.
 SUPPOSITORIES
• These are meant for insertion into the body cavities other than mouth.
They may be inserted in to rectum , vagina or urethra.
 POULTICES
• These are also known as cataplasams . They are soft viscous wet
masses of solid substances.
 PLASTERS
• These are solid or semi solid masses adhere to the skin when spread up
on cotton felt line or muslin as backing material.

10.  IPQC is concerned with providing accurate, specific, & definite
descriptions of the procedures to be employed from, the receipt of
raw materials to the release of the finished dosage forms.
 IPQC procedures are generally quick, simple and rapid tests or
inspection that carried out at on going manufacturing.
 Failure to meet in process control specification indicates either that
procedure were not followed or some factors out of control.
What is IPQC ?

11.  FPQC (Finished Product Quality Control) are tests that are
performed when manufacturing process is completed in order to
check qualitative and quantitative characteristics along with test
procedures and their acceptable limits by which the finished product
must comply throughout its shelf life.
 For qualitative and quantitative analysis of product
 Determines the test procedures and acceptance limit
 The product must comply with the acceptance limit for the approval
of complete batch manufactured.
What is FPQC ?

12. Classification of Quality Control tests
for Cream and Ointment
Universal
tests
Description
Identification
Assay
Impurities
Specific
tests
PH
Viscosity
Uniformity of weight
Microbial limit
Preservative efficacy test
Particle size
Sterility test
Performance
tests
Phase separation
Uniformity of container
In vitro release studies
Test of non irritancy
Spreadability

13. A. DESCRIPTION :
 This includes visual examination to identify changes in color,
separation, crystallization etc., in the final appearance of the product.
 The description should specify the content or label claim of the
product.
B. IDENTIFICATION :
 Qualitative identification of the active ingredient in the finished dosage
form.
 Methods : IR Spectroscopy
Raman spectroscopy
Chromatography
1. UNIVERSAL TESTS

14. C. ASSAY :
 The Quantity of drug present in unit weight or volume of ointment is
determined by- Spectrophotometric method
Titrimetric method
Microbiological assay
 For example: Salicylate ointment
D. IMPURITIES :
 Impurities arising from the degradation of the drug substance and those
arising during manufacturing process of the drug product should also be
assessed and controlled. (Process impurities , residual solvents , heavy
metals and other inorganic or organic impurities)

15. 2. SPECIFIC TESTS
Select A sample of 10 filled containers.
Clean and dry the outer surfaces of the
containers and weigh each container.
Remove quantitatively the contents from each
container.
If necessary, cut open the container and wash
each empty container with a suitable solvent.
Closure and other parts of the container are
retained.
A. UNIFORMITY OF WEIGHT :

16. Dry and again weigh each empty container together
with its parts which may have been removed.
The difference between the two weights is the net
weight of the contents of the container.
The average net weight of the contents of the 10
containers is NLT the labelled amount.
The Net weight of the contents of any SINGLE
CONTAINERS is NLT 91 % and NMT 109 % of the
labelled amount; where the labelled amount is 60 g or
less,
or NLT 95.5 % and NMT 104.5 % of the labelled
amount where the labelled is more than 60 G but
NMT 150g.

17. B. PARTICLE SIZE :
 Gently spread a small quantity of the Eye Ointment as a thin layer on a
microscope slide.
 Scan at least 50 representative fields.
 NMT 20 particles have a maximum dimension greater than 25 um,
NMT 10 particles have a maximum dimension greater than 50 um and
none has a maximum dimension greater than 100 um.
C. WATER CONTENT:
 Water activity test is generally formulation dependent, low water
activity reduces susceptibility to microbes.
D. ANTIOXIDANT CONTENT:
 Acceptance criteria, level of antioxidant necessary to maintain
product’s stabilityat all stages through its proposed usage and shelf
life.

18. E . TEST OF MICROBIAL CONTENT :
 Micro-organisms like Pseudomonas aeruginosa and Staphylococcus
aureus may contaminate the preparation and finally infect the skin.
 So ointments should be tested for the absence of such micro-organisms.
 Solutions of different samples of the preparation are made.
 Each sample is inoculated into separate volumes of 0.5 ml of rabbit's
plasma under aseptic conditions and incubated at 37ºC for 1-4 hours.
 No formation of the clot in the incubated mass indicates the absence of
the micro-organisms.
F. STERILITY TEST :
 Depending on the use of the dosage form the dosage form (Ophthalmic
preparations , products that will applied to open wounds or burned areas)
 Method A - Membrane Filtration
Method B - Direct Inoculation

19.  Method A- Membrane Filtration
Membrane filter - 0.22 um
Diluent - isopropyl myristate

20.  Method B - Direct Inoculation
 Incubate the inoculated media for NLT 14 days. Observe the cultures
several times during the incubation period. Observe the containers of
media periodically during the 14 days of incubation.
 If the test specimen is positive before 14 days of incubation, further
incubation is not necessary.
 For products terminally sterilized by a validated moist heat process,
incubate thetest specimen for NLT 7 days.
 NOTE - For ointments and oils that are insoluble in isopropyl myristate,
use Method B.
 No evidence of growth : passed the test for sterility
 Evidence of growth : retesting is performed with twice no. of sample
No growth - passed the test
if growth occurs - failed the test for sterility.

21. G. PRESERVATIVE EFFICACY TEST
 Using Pour plate technique the number of
micro-organisms initially presents in the
preparation is determined.
 Solutions of different samples of the
preparation. Mixed with tryptone azolectin
tween (tat) broth separately.
 Cultures of the micro-organisms are added
into each mixture Incubated.
 Then numbers of micro-organisms in each
sample are counted on 7th, 14th, 21st and 28th
days of inoculation.
 Bacteria : NLT 1.0 log reduction from initial 14
and no increase at 28 days.
 Yeast and Mold : no increase at 14 & 28 days.

22. H. pH DETERMINATION :
 Avoid irritation upon its application to the skin.
 GLASS ELECTRODE INSTRUMENT (pH meter).
 1 gm of the topical preparation is dissolved in 100 ml of distilled water
and stored for 2 hrs.
 pH measurement is done in triplicate and average values are
calculated.
J. SOLUBILITY :
 The contents should be soluble in 9 parts of water and in 1.7 parts of
hot water.
 The contents should be miscible with alcohol, ether and chloroform.

23. K. VISCOSITY DETERMINATION
(RHEOLOGY)
 The viscosity can be measured using
viscometers for non-Newtonian products.
 A bookfield viscometer can used to identify
the viscosity of the different topical
formulation.
 The tests were carried out at 21ºC.
 The spindle was rotated at various rpm such
as on 0, 0.5, 1 ,2 ,2.5, 4,5,10,20,50 and 100
all measurement were made in triplicate.
 There are used to ease of bottle pouring ,
squeezing from a tube container.

24. A. VISUAL INSPECTION - PHYSICAL APPEARANCE :
(ORGANOLEPTIC PROPERTIES)
3. PERFORMANCE TESTS

25. - CONSISTENCY : Should be smooth, no solid particles.
- TUBE EXTRUDABILITY :
• Aluminium collapsible tube with a nozzle tip of 5mm opening and
applies the pressure on tube by the help of finger.
• Tube extrudability determined by measuring the amount of ointment
extruded through the tip when a pressure was applied on tube .
B. SPREADABILITY :
 A sample of 1 g of semisolid was placed at the center of the glass
plate . Another glass plate was placed over it carefully. Above the
glass plates 2 kg weight was placed at the center of the plate avoid
sliding of the plate.
 The diameter of the semisolid in cm was measured after 30
minutes. The Experiment Was Repeated Three Times And The
Average Was Calculated.

26. C. UNIFORMITY OF CONTAINER :
 Carefully remove or cut off the bottom tube seal and make a vertical cut the
tube around the upper rim, open the 2 flaps and lay the flaps expose the
product.
 For multiple dose products that contain 5 g or more : Use single tube,
remove samples from top , middle and bottom of the tube and analyze.
 For multiple dose products that contain less than 5 g of product:
 If the product is fails acceptance criteria A, test two additional tubes
from the same batch following step 1 . And evaluate test results using
acceptance criteria B.
• Acceptance criteria A : all assay results are within the range of 90% -
110% of product label claim.
• Acceptance criteria B : no assay result is outside the range of 90% -
110% of the product label claim.

27. D. TEST FOR RATE OF ABSORPTION:
 The ointment should be applied over a
definite area of the skin by rubbing.
 At regular intervals of time, serum and
urine samples should be analyze for the
quantity of drug absorbed.
E. IN VITRO RELEASE TEST (RATE
OF PANRETRATION) :
 Franz diffusion cell - for studying
dissolution release through a cellophane
membrane.
 100 ml of dissolution medium
temperature of 32ºC and stirred at 100
rpm for one hour.
 Graph : Concentration versustime.

28. F. TEST OF NON-IRRITANCY
 In this test 24 human volunteers are selected. Definite quantity of
ointment is applied under occlusion daily on the back or volar
forearm for 21 days.
 Daily the type of pharmacological action observed is noted.
 No visible reaction or erythema or intense erythema with edema and
vesicular erosion should occur. A good ointment base shows no visible
reaction.
 MELTING POINT -Not less than 11ºC.

29.  METAL PARTICLE TEST FOR OPTHALMIC OINTMENT :
 Extrude completely the content of 10 containers
separately into flat bottom 60 mm petri dishes.
 Cover the petri dishes , heat at 85ºC for 2 hours. Slight
increase in temperature can be done to ensure complete
fluid state then cool slowly to solidify .
 Remove the cover and invert the petri dishes on the stage of microsope.
 Examine the entire bottom of petri dish for metal particles
 Count the metal particles of 50um or larger in any dimension .
 The requirement is met :
If total number of such particles in all 10 tubes does not exceed 50.
Not more than 1 tube contains more than 8 such particles .
 If the requirement is not met , repeat with 20 more tubes :
The test is passed if total number of particles of 50 um or larger in 30 tubes is
not more than 150. And not more than 3 containers contain more than 8 such
particles, individually.

30. 1. APPEARANCE:
 The medicated Gels can be examined physically for appearance like
clarity, colour and presence of any particle.
2. HOMOGENEITY :
 All developed gels were tested for homogeneity by visual inspection
after gel set in container for their appearance and presence of any
aggregate.
3. pH : Standard pH of gel is 5 to 5.5.
Evaluation of Gels

31. 4. SPREADABILITY:
 Spreadability is measured by spreading 0.5 g Gel on a circle of 2 cm
diameter on a glass plate. Then a second glass plate is placed. 1/2 kg
weight placed on the upper glass plate for 5 minutes. Finally diameter of
circle spreading is measured.
S = ML/T
where , M= weight of an upper side
L= length of circle/ diameter
T= time in minute
5. EXTRUDABILITY :
 Extrude at least 0.5 cm ribbon of gel in 10 seconds.

32. EVALUATION OF
SUPPOSITORIES
A. Appearance
B. Uniformity of weight test
C. Uniformity of content test
D. Melting rang test
E. Liquefaction test
F. Breaking test
G. Dissolution test

33. A. APPEREANCE :
Surface appearance and colour can be verified usually to assess absence
of fissuring, absence of fissuring, absence of pitting, absence of exudation,
absence of migration of the active ingredients.
B. UNIFORMITY OF WEIGHT TEST (WEIGHT VARIATION) :
 To perform this 20 suppositories are weighed and average weight is
calculated.
 Then each suppository is weighed individually and weight noted.
 No suppository should deviate from the average weight by more than
5%except that two should not deviate by more than 7.5%.
 The weight variation may result if some cavities are under filled and
other are overfilled.

34. C. UNIFORMITY OF CONTENT :
 In order to ensure content uniformity , individual suppository must be
analyzed to provide information on dose to dose uniformity.
 Assay 10 units individually as directed in assay of individual monograph.
 For determination of drug content the suppositories were dissolved in 100
ml phosphate buffer of pH 7.4 by stirring through magnetic stirrer slowly
at 37ºC for 1 hr.
 After the solution was filtered and the filtrate was diluted suitably and
absorbance was measured against blank at 371 nm.
D. MELTING RANGE TEST :
 This test is also called the macro melting range test and is a measure of
the time it takes for the entire suppository to melt when immersed in a
constant-temperature (37ºC)water bath.
 In contrast, the micro melting range test in the melting range measured in
capillary tubes for the fat base only.

35.  The suppository is completely immersed in the constant water bath, and
the time for the entire suppository to melt or disperse in the surrounding
water is measured.

36. E. LIQUEFACTION or SOFETNING
TIME TEST :
 It consists of a U-tube partially
submersed in a constant- temperature
water bath.
 A constriction on one side hold the
suppository in place in the tube.
 A glass rod is placed on top of the
suppository and the time for the rod
to pass through to the constriction is
recorded as the softening time.
 This can be carried out at various
temperatures from 35.5 to37ºC, as a
quality control check.

37. F. BREAKING TEST (HARDNESS):
 The breaking test is designed as a method
for measuring the fragility or brittleness of
suppositories.
 The suppository is placed in the chamber.
 Add 600 g , leave it for 1 min.
 If not broken, add 200 g every 1 min. until
the suppository is broken.
 The weight at which the suppository
collapses is the breaking point, or the
force that determines the fragility or
brittleness characteristics of the
suppository.

38. G. DISSOLUTION TESTING :
 Testing for the rate of in vitro release of
drug substances from suppositories has
always posed a difficult problem, owing to
melting, deformation, and dispersion in the
dissolution medium.
 Two types of apparatus are available for
testing :
 Suppository dialysis cell (natural
membranes)
 Stationary basket : rotating paddle
apparatus (USP dissolution apparatus)

39. 1. Indian Pharmacopoeia, Government of India, Ministry of Health and
family Welfare , Indian Pharmacopoeia commission , Ghaziabad 2018,
Volume -1 and 2.
2. Lachman L., Lieberman H.A and Kanig J.L, “Theory & Practice of
industrial pharmacy”, Lea & Febieger, Philadelphia 4th edition 2016.
3. “The United States Pharmacopoeia. The National Formulary” Rockville
Md : United States Pharmacopeial convention, inc., 2019.
4. Review Article on Ointment, International Journal of Pharmacy and
Pharmaceutical Research, Human Journals, September 2015 Vol.4, Issue
2.
5. Chauhan L, Gupta S, Creams: A Review on Classification, Preparation
Methods, Evaluation and its Applications, Journal of Drug Delivery and
Therapeutics. 2020; volume10 , issue5-s 281-289.
References

40. THANK
YOU