OBJECTIVE
To lay down the Calibration procedure for the dissolution test apparatus (Make: Electrolab, Model: EDT-08LX) for better and error-free use.
SCOPE
This procedure is applicable for dissolution test apparatus (Make: Electrolab, Model: EDT-08LX) located in the Quality Control Laboratory
RESPONSIBILITY
Execution: Chemist and above - QC department.
Checking: Asst. Manager and above - QC department.
FREQUENCY
Calibration shall be done every six months and after maintenance or replacement of spare parts.
PROCEDURE
Calibration of the Dissolution Apparatus is done in the following steps.
- Physical Verification Parameter
- Performance Verification Parameter
Physical Verification Parameter
WOBBLING:
- Switch ‘ON’ the mains.
- Fix the wobble meter near the shaft for which the wobble is to be measured.
- Run the system at 50 RPM for 1 minute, observe the wobble on the Wobble Meter, and note the wobble reading as per Attachment-I. (Calibration Record of Dissolution Test Apparatus - Physical Verification, 1. Wobbling).
- Repeat the procedure by setting 150 RPM.
Acceptance Criteria:
a. For Apparatus-I (Basket): ± 1mm
b. For Apparatus-II (Paddle): ± 0.5 mm
TEMPERATURE:
- Fill each bowl/vessel with water (900 mL) and set the temperature to 37°C.
- Run the system for 45 minutes. Measure the temperature of the water in the jars using a calibrated thermometer.
- Record the observations as per Attachment I. (Calibration Record of Dissolution Test Apparatus - Physical Verification, 2. Temperature).
Acceptance Criteria: 37.0 ± 0.5˚ C
TIME:
- Set the time to 30 minutes.
- Start the stopwatch when the run starts.
- Stop the stopwatch when the run ends.
- Record the set time and the time shown by the stopwatch as per Attachment-I. (Calibration Record of Dissolution Test Apparatus - Physical Verification, 3. Time).
- Repeat the above procedure by setting the time to 60 minutes.
Acceptance Criteria: The difference between the set time and the time shown by the Calibrated stopwatch shall not be ± 36 seconds for 30 minutes and ± 72 seconds for 60 minutes (± 2% of the set time).
RPM:
- Lower the basket/Paddle by pressing the “Down” Lift key.
- Set 50 RPM and press start RPM; the rotation will start.
- Measure the rotation by using a calibrated tachometer, Repeat the above procedure by setting 100 and 150 RPM.
- Record the observations as per Attachment I. (Calibration Record of Dissolution Test Apparatus-Physical Verification, 4. RPM).
Acceptance criteria: ± 1 RPM of the set value.
JAR CENTERING:
The jar centering is carried out with the help of Vernier Caliper, and the Jar Centering is given below:
Where:
- X1 → Distance along with X-Axis from the right side of a glass jar to the Paddle/basket.
- X2 → Distance along with X-Axis from the left side of a glass jar to the Paddle/basket.
- Y1 → Distance along with Y-Axis from the front side of a glass jar to the Paddle /basket.
- Y2 → Distance along with Y-Axis from the back of a glass jar to the Paddle/basket.
- Repeat the procedure for both the paddle & basket and Record the observations as per Attachment-I. (Calibration Record of Dissolution Test Apparatus-Physical Verification, 5. Jar Centering).
Acceptance Criteria: Not more than 2 mm.
PADDLE/BASKET DEPTH:
- Measure the distance between the inside bottom of the vessels and the bottom of the paddle /basket by depth gauge.
- Repeat the procedure for individual eight jars using the paddle and then the basket and Record the observation as per Attachment-I. (Calibration Record of Dissolution Test Apparatus - Physical Verification 6. Paddle & Basket Depth).
Acceptance Criteria: The distance between the inside bottom of the vessels and the bottom of the paddle/basket should be 25 ± 2 mm.
Performance Verification Parameter
DISSOLUTION CONDITIONS:
Apparatus: Type-1 (Basket) and Type-2 (Paddle)
Medium: 500 mL Purified Water
Medium Temp.: 37° ± 0.5°C
Time: 30 Minutes
RPM: 50 RPM
Wavelength: 240 nm
Standard preparation:
Take 10 mg of Prednisone RS in a 100 mL volumetric flask, add 5 mL of ethanol, and sonicate to dissolve and make up to the volume with purified water, Further dilute 5 mL of this solution to 25 mL with purified water.
Sample preparation:
After reaching the set temperature, place one Prednisone tablet in each six dissolution vessels & run the test. After the completion of the test, withdraw the sample from each vessel with a cannula from the zone midway between the surface of the dissolution medium and the top of the rotating basket/paddle and not less than 10 mm from the wall of the vessel. Filter the solution with a 0.45 µm porosity filter. Take the absorbance of the standard and sample solution at 240 nm.
Repeat the procedure for another set of six tablets.
Calculation:
- Record the observation as per Attachment II. (Calibration Record of Dissolution Test Apparatus-Performance Verification)
Acceptance Criteria: Refer to COA of the current lot of prednisone tablets.
ATTACHMENTS
Attachment-I - Calibration Record of Dissolution Test Apparatus (Physical Verification)
Attachment-II - Calibration Record for Dissolution Test Apparatus (Performance Verification Test)
REVISION HISTORY
Nil
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