pharmceutical analysis m.pharm pharmaceutical validation

1. KARNATAKA COLLEGE OF PHARMACY
Seminar topic: QUALIFICATION DISINTEGRATION
APPARATUS
By: KAVANA BB
1ST SEM M Pharm
Subject : PHARMACEUTICAL VALIDATION
DEPARTMENT OF PHARMACEUTICAL ANALYSIS SUBMITTED TO:DR.C .SREEDHAR
PROFESSOR & HOD
DEPARTMENT OF PHARMACEUTICAL ANALYSIS
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2. INTRODUCTION
• Disintegration testers are widely used to
measure the quality of the oral dosage form like
tablets and capsules.
• Disintegration testers are comprised of a
reciprocating arm that drops in and out of a
vessel. This vessel sits inside a heated water bath
which mimics the human body temperature.
Inside the vessel is the test media, which has a
ph. level similar to that of the human stomach.
This crates the simulated environment of the
human body.
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3. • Attached to the moving arms of all disintegration testers is a
basket. It is here that the tablets/samples are held. Each basket
can contain up to 6 tablets, separated into glass vials. There are
also 3-vial baskets available for bigger samples.
• At the bottom of the vials are metal mesh disks, which
ultimately provide the crucial evidence that the sample either
has, or has not, disintegrated correctly.
• The tablet/sample is placed inside the vial, on top of the mesh,
and a small disc is placed above the tablet to stop it from
floating to the surface of the media, keeping the sample
submerged.
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4. • The reciprocating arm raises and lowers the basket in and out of the vessel
for fifteen minutes, and during this time the friction of the test media on
the sample initiates the disintegration. This movement mimics the flow
and friction that would be experienced inside the human body. Once
fifteen minutes has accrued, the moving arm is halted and raised out of the
vessel for inspection.
• If there is residue left on the mesh, the test has failed. If there is no residue
present, then the test is recorded as a pass. If there is no residue on the
mesh disk, then it means the sample has crumbled into a powder and
fallen through the mesh, confirming a successful disintegration.
• USP regulations stipulate that all samples must disintegrate in under 15
minutes. The USP also specifies the mechanical requirements of all
disintegration testers, including the speed of the moving arm, the
dimensions of the basket, the size of the vials and mesh, and the ph. level
of the test media and water tank temperature.
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6. Validation of Disintegration Test Apparatus
The Important parameters calibrated are
 Number of Strokes / min
 Stroke height
 Temperature
 Basket’s lower most position
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7. Number of Strokes / min
Record the frequency of moving up and down of the basket rack
assembly in a given time as shown below
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8. Record the frequency (of moving up and down) manually with respect
to time
Do not stop the instrument in between the operation
Measure the frequency initially and after each 15 minutes interval
from the start, for 5 minutes (each)
Record 5 readings
Divide the observed reading by five and note as frequency of moving
up and down per minute
Perform the test for both the basket rack assembly positions (Side A &
Side B) individually
Acceptance Criteria :The number of cycles per minute should be 30 ±
2 throughout the period of operation.
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9. Stroke height
Attach the basket rack assembly firmly
Attach white paper without touching on the instrument, parallel to the path
of the arm of basket rack assembly
Select one point on the horizontal arm of the assembly and mark the same
on the paper when assembly is not moving and at its highest position
Start the instrument by pressing Start/Stop key and followed by pressing the
respective timer key
As soon as assembly reaches the lowest position, mark the same point again
on the paper (while doing this activity take time to decide the exact lowest
position and then mark)
Measure the distance between two marks using calibrated ruler
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10. Perform the test initially, after 60 minutes from start and same after
120 minutes.
Perform the test for both basket rack assembly positions (side A &
side B) individually
Acceptance Criteria : The stroke height should be 55 ± 2 mm
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11. Temperature
Fill the beaker with water
Set the temperature to 37 ˚C
Attach the basket rack assembly and start the oscillation
Insert the calibrated thermometer in one of the tubes of the basket rack assembly
Wait till the temperature reaches between 36 ˚C to 38 ˚C
Start recording the readings
Record the temperature reading initially and after each 15 minutes interval upto
120 minutes from the start
Perform the test for both the basket rack assembly positions individually
While performing the test, do not keep thermometer inside the basket rack
assembly constantly. But insert 2 to 3 minutes prior to the measurement to give
stable reading
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12. Acceptance Criteria : The temperature should remain within 37
± 1˚C through out the operation
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13. Basket’s lower most position
The lower most position of the basket is measured
The values are noted down in mm
• Acceptance Criteria : The temperature should remain within 37 ± 1˚C
through out the operation
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14. Design Qualification
Design qualification should provide
documented evidence that the design
specifications were met.
Few specifications about the Basket rack
assembly etc., are mentioned in USP
So the manufacturer should also meet the
GMP requirements.
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15. Installation Qualification
Installation qualification should provide documented evidence that the
installation was complete and satisfactory.
The purchase specifications, drawings, manuals, spare parts lists and
vendor details should be verified during installation qualification.
Control and measuring devices should be calibrated.
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16. Conditions :
 Clean, well ventilated
 Well lit
 Free from rodents
 Free from microbial contaminants
 Air should free from pollutants
 Have sufficient space around
 Not to be kept very adjacent to any other equipment (especially
should be away from those equipments producing heat)
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17. The base unit is fitted on the surface where it has to be placed
Water bath is placed & heating coils are placed in the water bath and
fixed
Water bath cover is fitted over the water bath
Place the beakers in the space provided through the water bath cover
Glass tubes / plastic tubes are placed in the basket (Basket rack
assembly)
Water bath is first filled with water and then beaker is filled with
water
Water is filled upto the mark in both the waterbath and beakers
In the beaker only 800 - 900 ml of water should be filled. Once the
water is filled upto the mark, the basket assembly is lowered into the
beaker
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18. Switch on the mains
On the switch provided at the rear panel
Make sure the Red light indicator is on
Suspend the basket rack assembly in 1000 ml beaker containing specified liquid
medium
Switch on the heater thermostat and adjust temperature to the liquid bath at 37˚C
The green light indicator will be on and off and the temperature is maintained
Now add the number of samples (as specified in the monograph) in the cylindrical
glass tubes provided in the basket rack assembly
Place the glided disks where applicable
Operation procedure
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19. The oscillation can be turned on
Now the tablet will be disintegrated as per the USP specification of the specific tablet
The time when the basket rack assembly having tablet is suspended in the beaker
containing specific buffer is noted down as T1
The time when the disintegrating tablet has totally passed out from the glass tube
having mesh is noted down as T2
T2 - T1 = T3 (Difference in the disintegration time)
T3 is the Disintegration time of the particular tablet
As soon as the disintegration test is performed the equipment is turned off
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20. Performance Qualification
Performance qualification should provide documented evidence that utilities,
systems or equipment and all its components can consistently perform in
accordance with the specifications under routine use.
Test results should be collected over a suitable period of time to prove consistency.
(Calibration)
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21. •THANK YOU
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