Dissolution Apparatus Calibration procedure:
There are 2 types of dissolution calibration performed in the pharmaceutical industry, 1. Physical calibration and 2. Chemical calibration.
In physical calibration, there are 11 parameters and chemical calibration is performed by using a Prednisone tablet.
Dissolution Apparatus Calibration Procedure for physical parameters:
- Basket and paddle depth
- Base plate level
- Shaft vertically
- Vessel vertically
- Centering
- Rotation per minute (RPM)
- Temperature
- Time
- Wobbling
- Volume accuracy and replacement volume accuracy
- Vibration Check
The dissolution apparatus calibration procedure in pharmaceuticals is as below.
Basket and Paddle depth:
- Attach the basket and paddle to the shaft.
- Place the depth gauge on the bottom of the vessel. All the paddles are lowered into the vessel until those touch to the top of the depth gauge.
- Measure the depth gauge of the peddles in the respective vessels.
- Similarly, measure the basket depth.
Acceptance Criteria:
The Depth should be 25 ± 2 mm for both apparatus 1 and apparatus 2.
Base Plate Level:
- Fill the water bath up to the mark without a vessel.
- Measure the inclination on the base plate in two orthogonal directions by using calibrated digital degree protractor.
Acceptance Criteria:
Base plate inclination shall be not more than 0.5°.
Shaft Vertically:
- Verify the verticality of the stirring elements by using a calibrated digital protractor.
- Measure the verticality for each stirring element in two orthogonal positions.
- The ideal reading obtained on the vertical surface shall be 90.0°.
Acceptance Criteria:
The deviation shall be not more than 0.5°.
Vessel Vertically:
- Verify the verticality of the vessel by using a calibrated digital protractor.
- Measure the verticality for each vessel in two orthogonal positions oriented at 90.0°. around the vessel axis.
- Measurement shall be made on the vessel’s inner surface.
- The ideal reading obtained on the vertical surface shall be 90.0°
Acceptance Criteria:
The deviation shall be not more than 0.5°.
Centering:
- Centering shall be evaluated for the stirring elements placed within the vessel as it would be during the test.
- A mechanical or digital centering device that measures inside the vessel is required to perform this check.
- Measure the centering of the vessel with respect to the shaft at two different positions using centering measured using an inside divider to obtain a distance and measuring a distance with the Vernier caliper or micrometer at top of the rim of the vessel and just above the paddle or basket level in the vessel.
- Measure the distance from the shaft to the inner vessel wall at four locations equally spaced around the vessel and not more than 2 cm below the vessel flange.
- Repeat the same procedure of the above two points to check centering of other vessels.
Acceptance Criteria:
The difference between the smallest and largest reading shall not be more than 1.0 mm from the center line.
Rotation Per Minute (RPM):
- Set the RPM to 50
- Mark each paddle holder with radium paper, and count the revolutions by using calibrated Tachometer.
- Repeat procedure for 100 RPM also.
Acceptance Criteria:
The RPM shall be ± 1 for the set value.
Temperature:
- Fill each vessel with 500 ml purified water and set RPM as 50.
- Set the temperature to 37°c and with intervals of 30 minutes and 60 minutes.
- Record the temperature of the individual bowl by using calibrated tachometer at the beginning, middle (30min), and end (60min) of the run.
Acceptance Criteria:
- The difference between the set temperature and the observed temperature shall not be more than 0.5°c
- The temperature measured by the equipment in all the vessels shall be within the range of 0.4°c at a specified time interval.
- The difference between the temperature shown by the external thermometer and equipment should be not more than 0.5°c.
Time:
- Set the timer for 30 minutes.
- Simultaneously start the timer and calibrated stopwatch.
- When the beep sound starts, check the time on a stopwatch and record it.
- Follow the same procedure to calibrate 45 minutes intervals.
Acceptance Criteria:
- The difference shall not be more than ± 36 seconds for 30 minutes.
- The difference shall not be more than ± 54 seconds for 45 minutes.
Wobbling:
- For Paddle: Fix the calibrated dial gauge about 1 cm above the paddle blade.
- For Basket: Fix the calibrated dial gauge at the bottom of the basket rim.
- Run the system with 25 RPM and observe the wobble on a dial gauge.
Acceptance Criteria:
The deflection of the probe tip shall be not more than 0.039 inches (1 mm).
Volume Accuracy and Replacement Volume Accuracy:
- Create a method to carry the volume calibration and sample replacement.
- Ensure Recycle and media replacement is “ON” in this method.
- Set up to execute and run “Empty” auto action.
- Mark and weigh the empty test tubes (W1) in Row 1 and record the weights.
- Mark and partially fill individual beakers or vials with purified water for each channel.
- Weigh each beaker or vial with water and record the weights (W2).
- Ensure the replacement lines are placed in a suitable reservoir with sufficient purified water in it for total replacement volume.
- Position each sampling probe in the respective beaker or vial and start the test.
- When the system is ready to collect the first sample into the first row, the carriage will move to the first row.
- At the completion of the sample collection, the system will go through the purge action and then execute the replace action.
- At the end of the “Replace” operation, the system will display active immediately upon the display of the active status, remove the sampling probe from the individual beakers or vials and transfer them all into one beaker filled with purified water.
- Reweigh all the individual beakers or vials to record the data (W3).
- Reweigh the test tubes with the sample and record the weights (W4).
- Media sample volume = (W4-W1) x 1.003996 (at 25° c).
- Media replacement volume = (W2-W3) x 1.003996
Acceptance Criteria:
- 10 ml ± 0.5 ml for sampled volume.
- Replacement volume should not differ by 1.0 ml with respect to sample volume.
Vibration Check:
- Fill each vessel with 900ml of purified water and set RPM as 100.
- Place the digital or analog vibration meter on the base plate.
- Check the vibrations at 4 corners.
Acceptance Criteria:
For Information.
This is the Dissolution Apparatus Calibration procedure and physical calibration parameters in pharmaceuticals.
Also read:
- OOS Investigation checkpoints
- QA Interview Question and answer
- Computer system validation in pharma
- What is data integrity and Alcoa Plus?
- What are the factors for cleaning validation?
- Preparation and standardization of KOH
Refer YT channel: Pharmabeej
