Quality Con

trol tests
of Solid Dos
age Forms
7 th
Semester, Se
Instructor: ction A, B an
Ms. Maryam dC
Professor, F Shabbir, Ass
aculty of Ph istant
armacy
 Quality Control Tests
0 The Quality control tests on solid-dosage form may
include:

1. Physical Tests
2. Chemical Tests
3. Microbiological Tests
4. Biological Tests
 Thickness

Diameter

Hardness

Physical Tests Friability

Loss on Drying (LOD)

Weight Variation

Flow properties
 Drug Content

Chemical Tests Disintegration

Dissolution

Microbiological
Biological Assay
Assay

Performed on Performed on living

microorganism organism like animals
 Thickness and Diameter

Tablet Thickness Tablet Diameter

0 n = 10 0 n = 10
0 Apparatus used for 0 Apparatus used for
measurement: measurement:
Vernier caliper and Vernier caliper and
micrometer micrometer
screwguage screwguage
0 Un-official tests 0 Official tests
Thickness vs.
Diameter
The Figure signifies the
difference between the
thickness and diameter of the
tablet.

Here, d is the diameter and e is

the thickness of the tablet.
Official Limit of Diameter as per USP
criteria

0 The deviation of individual unit from the mean

diameter should not exceed ± 5% for tablets with
diameter of less than 12.5 mm

0 The deviation of individual unit from the mean

diameter should not exceed ± 3% for diameter of 12.5
mm or more.
 Manual Vernier Caliper
Used for the estimation of thickness, diameter and depth

Thickness/ Diameter = Main Scale (cm) + Vernier Scale reading*Least count (mm)
Convert to same Unit : cm or mm
Manual Vernier Caliper
Example
 Test Example
Main Scale Vernier Least Percentage Within
Tablet #
(cm) Scale (mm) Count deviation Limit
1 1.2 40 0.01 4.62% No

Vernier Scale reading = 40*0.01 = 0.40 mm

Convert it into cm = 0.40/10 = 0.04 cm

Diameter = 1.2+0.04 = 1.24 cm

Average diameter = 1.3 cm (Assumed in this case)

Percentage deviation = (1.3-1.24)/1.3 *100

 Hardness

Tablet hardness testing is a laboratory method which is applied to

measure the breaking point of a tablet.
Tablet hardness testers function on the basis that it requires a
specific quantity of force to fracture a tablet.

Tablet hardness testing makes sure that solid tablets are hard enough
to sustain mechanical strains during various situations like storage
and packaging, delivery and handling by the user, among others.
 Hardness

To determine the tablet disintegration

An exceedingly hard tablet could designate excessive bonding
possibilities between excipients and active ingredients, which can
hinder proper disintegration of the tablet required for a correct
dosage.
Conversely, a softer tablet could indicate weak bonding and may
result in premature dissolution when consumed by the patient.
 Hardness

To determine tablet handling

A soft tablet may not sustain the handling and could crack or chip
during the successive processing phases of production,
These many include coating and packaging and during
transportation.
Thus, hardness is also related to friability.
 Hardness

To determine the material ingredients

Knowing the mechanical features of a solid-dose tablet can give
important information necessary for optimizing material ingredients.
The nature of active constituent(s), the kind of binder used, and the
composition of the constituent(s) in the tablet will impact on the
hardness of the tablet.
 Hardness

Instruments to determine the hardness of the tablet

1. Pfizer Hardness Tester

2. Monsanto Tester
3. Strong-Cobb Tester
4. Erweka Tester
Monsanto harness tester: Diagrammatic representation

Monsanto harness tester: Actual Image

 Hardness

Units to determine the hardness of the tablet

Kilogram (kg) – SI system recognizes kilogram as the main unit of mass.

Newton (N) – This is the SI unit of force; the measure for tablet hardness tester
machines. 9.807 Newton = 1 kilogram (at earth surface gravity).
Pound (lb) – Basically pound is a unit of force though you can as well use it for
mass under earth gravity. It is not an SI unit. 2.204 pounds = 1 kilogram.
Kilopond (Kp)
Strong-Cobb (SC) –1 SC equaled about 7 Newton or 0.7 kilograms of force.
 <1216> Friability
It describes the tendency of a solid substance to break into smaller
pieces under stress or contact with other surfaces.
Also known as ‘Drop test’ or ‘Abrasion test’.
 Body
Drum
Lid/ cover

Display – Time
and rpm
Drum –
Removable, Screw – Untighten to
Polished remove cover/ lid
surface,
Synthetic
polymer Curved
Projection
 Sample size
For tablets with a unit mass equal to or less than 650 mg, take a
sample of whole tablets corresponding to 6.5 g.

Example: 300 mg weight unit tablet

1 tablet = 300 mg, 6500 mg will correspond to how many tablets.

Number of tablets taken for friability = 6500/300 = 21.66

We will take approx. 22 tablets for the test

OR
For tablets with a unit mass of more than 650 mg, take a sample of
10 whole tablets.
 Procedure

1. The tablets should be carefully dedusted prior to testing.

2. Accurately weigh the tablet sample, and place the tablets in the
drum.
3. Rotate the drum 100 times, and remove the tablets.
4. Remove any loose dust from the tablets as before, and
accurately weigh.

Friability (%) = Initial weight – Final Weight x100

Initial weight
 Acceptance criteria
0 The percentage friability should be less than 1% (USP) or 0.8%
(BP).

0 If cracked, cleaved, or broken tablets are present in the tablet

sample after tumbling, the sample fails the test.

0 If the results are doubtful or if the weight loss is greater than the
targeted value, the test should be repeated twice and the mean of
the three tests determined.

0 Effervescent tablets and chewable tablets may have different

specifications as far as friability is concerned. In the case of
hygroscopic tablets, an appropriate humidity controlled
environment is required for testing.
 Powder flow properties
The powder flow behavior during die filling is governed by a combination of a
number of factors:
1. Powder characteristics (particle size, size distribution, density, shape, and
surface properties),
2. Apparatus features (shoe and die design), and
3. Operating conditions (shoe kinematics, the absence or presence of air, suction,
vibration, agitation, aeration, humidity, and temperature).
4. Understanding the effects of these factors is crucial for the selection of
operating parameters and the control of the filling process.
Pharmaceutical secondary process selection based on powder
compressibility and powder flow—qualitative diagram.
 Estimation of bulk density and tapped density

Bulk density Tapped density

1. Take a graduated measuring
1. After recording the reading for
cylinder.
bulk density, tap the measuring
2. Pour a defined amount of
cylinder 100 times.
powder (mass in grams) into
2. Tapping should be slight.
the cylinder.
3. Record the reading on the
3. Record the reading on the
measuring cylinder.
measuring cylinder.

Bulk Density = Tapped Density =

mass/volume mass/volume
Units = g/ml Unites = g/ml
Estimation of bulk density and tapped density
Carr’s Index
Carr’s index = (Tapped density – Bulk density) / Tapped density *100

Hausner Ratio
Hausner ratio= Tapped density/ Bulk density
 Estimation of Angle of repose

Angle of repose is a characteristic related to interparticulate friction or

resistance to movement between particles.
According to the USP, it is the constant, three-dimensional angle
(relative to the horizontal base) assumed by a cone-like pile of material
formed by any of several different methods.
Due to the high dependence of angle of repose measurements on testing
conditions, angle of repose is not a very robust means of quantifying powder
flow.
Angle of repose setup: Angle of repose setup: Diagrammatic representation
Actual image

Acceptance Limits

Formula
tanƟ = height/radius

Where
radius = diameter/2
 Weight Variation Test

Weight of solid dosage form = API + Excipients

Thickness

Diameter

Drug content of solid dosage form = amount of API

 Procedure

1. The tablets (n=20) randomly selected from the batch.

2. Individually weigh each tablet on the weighing balance.
3. Calculate the average.
4. Estimate the percentage deviation.
5. Identify the limit of acceptance applicable on the solid dosage form.
6. Infer whether the batch is accepted or rejected.

Deviation (%) = (Average weight – Individual weight)/ Average weight *100

 Acceptance limits/ Limit of acceptance (BP)

If 20/20 falls within the 1st limit of acceptance: Accept the batch
If 19/20 or 18/20 falls outside the 1st limit but within the 2nd limit of acceptance:
Accept the batch

If 17/20 or falls within the 1st limit of acceptance: Reject the batch
If any tablet falls outside the 2nd limit: Reject the batch
 Limit of acceptance for tablets

Limit of acceptance for solid dosage forms

 Test Example
Weight of tablet Percentage
Tablet # Within Limit
(mg) deviation
1 510 -2.0% Yes

Average diameter = 500 mg (Assumed in this case)

Percentage deviation = (500-510)/500 *100

As the weight of the tablet falls in the category of ‘More than 250 mg (BP)’ and
‘More than 325 mg (USP), thus a deviation of ±5% is allowed.
The tablet falls within the ALLOWED percentage deviation.
Hence, the batch is accepted