*1.
Open Capillary Method*
- A small sample of the suppository is placed in a capillary tube.
- The tube is then heated gradually in a water bath or heating block.
- The temperature at which the sample starts to melt and becomes
transparent is recorded as the melting point.
*2. Drop Point Method*
- A suppository sample is placed in a specialized apparatus.
- The sample is heated gradually, and a small weight or probe is placed on
top.
- The temperature at which the sample softens and drops or deforms is
recorded as the melting point.
*3. Sliding Test*
- A suppository is placed on a temperature-controlled surface, such as a hot
plate or water bath.
- The surface is gradually heated, and the temperature at which the
suppository starts to soften and slide or deform is recorded.
- This method simulates the conditions in the rectum or vagina.
*4. Differential Scanning Calorimetry (DSC)*
- A small sample of the suppository is placed in a DSC instrument.
- The sample is heated gradually, and the instrument measures the heat flow
and temperature changes.
- The melting point is determined by analyzing the resulting thermogram,
which shows the endothermic peak corresponding to the melting transition.
Breaking Test (Hardness test)
Purpose:
This test applied to suppositories and passeries based on fatty excipients. It
is not suited to suppositories and passeries based on hydrophilic excipients
such as gelatin-glycerol mixture.
Hardness indicates the maximum force which the suppository can withstand
during storage, packaging and hardening. This test is design to check:
Hardness
Fragility
Brittleness
Apparatus
A therrnostaled chamber closed in front by a glass window and containing a
device that is to hold the suppository or passery.
Two opposite jaws, the upper jaw descending vertically toward the lower jaw.
The crushing surfaces of the jaw are flat perpendicular, to the direction of
movement and larger than zone of contact with the suppository or passery
A plastic sample holder is fixed in the center of the jaw (half a holder in cach
jaw).
The upper jaw (top pressure block) is connected to suspension to which can
be added each of which weight 200g. The initial mass of the device is 600g.
Crushing of the sample is carried out by successive adding 200g disc to the
initial mass of 600g.
Procedure
1. The suppository is placed in the instrument
2. Add 600 g; leave it for one min. (use a stop watch)
3. If not broken, add 200 g every one min, until the suppository is broken.
Calculations: The hardness of the suppository is calculated by adding the
weights together.
Limit: 1.8-2kg If the suppository is broken before the end of the last nin, the
last weight is canceled
4. Liquefaction time (Softening time test)
“The conversion of solid or gas into liquid is called Liquefaction.” Liquefaction
testing provides information on the behavior of a suppository when subjected
to the maximum temperature of 370 and pressure to release API.
The test commonly used is Krowzynski’s method, which measure the time
required for the suppository to liquefy under pressure similar to those found
in the rectum (approx. 30g) in the presence of water at 37oC
In general, the liqucfaction should take no longer than 30 minutes.
Krowzynski’s method
Apparatus I
The apparatus consists of a 16 mm diameter glasa tube, 235 mm long with
an approximately 6 mm diameter
Reduction at the base
One end is blocked with a small rubber stopper to facilitate cleaning after
use.
A thermostat graduated in lengths of a centigrade is used.
The tube and thermometer are held in place by means of a large ruhher
stopper with two holes in a 225 mm long supper tube with a 50 mm
diameter, filled with laterali lateral tubes to allow the water at 3700 from a
constant temperature water
Bath to circulate.
Apparatus II
Another apparatus equipped with a 30g glass stem 180mm long and 9mm
wide. The base has a ring form with a 14mm diameter.
The ring of the stem has a cuneiform shape opening to allow the melted
excipient to escape upwards during the test
At a distance of approximately 100mm from the ring, three glass projections
supports the stem in a vertical position in a tube.
LIQUEFACTION OR SOFTENING TIME TEST
Liquefaction testing provides information on the behavior of the suppository
when subjected to a maximum temperature of 37°C.
This test measures the time required for a suppository to liquefy under
pressures similar to those found in rectum (approximately 30g) in the
presence of water at 37°C.
In general liquefaction should take no longer about 30 minutes.
LIQUEFACTION OR SOFTENING TIME TEST
In this test a U tube is partially immersed in a constant temperature bath and
is maintained at temperature between 35°C to 37°C.
There is a constriction in the tube in which the suppository is kept and above
the suppository, a glass rod is kept.
The time taken for the glass rod to go through the suppository and reach the
constriction is known as the liquefaction time or softening time.
Another apparatus is there for finding softening time which mimics in vivo
conditions.
It uses a cellophane tube tied to both ends of a condenser with each end of
the tube open, and temperature is maintained by water circulation.
Time taken for the suppository to melt is noted. This apparatus can also be
used to determine the melting point of suppositories made with both water-
soluble and water-insoluble bases.
This can be accomplished by increasing the temperature of water at a set
rate, for example, one degree every 10 minutes until the suppository melts.
