SOP for Calibration of Dissolution Apparatus

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 Dissolution Apparatus is done in following steps. 

1. Physical Verification Parameter 
2. Performance Verification Parameter  

Physical Verification Parameter 

WOBBLING: 

• Switch ‘ON’ the mains. 
• Fix wobble meter near to shaft for which wobble is to be measured. 
• Run the system with 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 37.0 °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 

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TIME:

• Set the time to 30 minutes. 
• Start the stop watch when run starts. 
• Stop the stop watch when the run ends. 
• Record the set time and the time shown by stopwatch as per Attachment-I. (Calibration Record of Dissolution Test Apparatus - Physical Verification, 3. Time). 
• Repeat the above procedure by setting time 60 minutes. 
• Acceptance Criteria: The difference between set time and the time shown by 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 “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 set value. 

JAR CENTERING:

The jar centering is carried out with the help of Vernier Caliper, and calculate the Jar Centering as given below: 

Where: 

X1 → Distance along with X-Axis from right side of glass jar to the Paddle/basket. 

X2 → Distance along with X-Axis from left side of glass jar to the Paddle/basket. 

Y1 → Distance along with Y-Axis from front side of glass jar to the Paddle /basket. 

Y2 → Distance along with Y-Axis from back side of 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 inside bottom of the vessels and bottom of paddle /basket by depth gauge. 
• Repeat the procedure for individual eight jars using the paddle 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 inside bottom of the vessels and bottom of 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 cannula from the zone midway between the surface of dissolution medium and the top of the rotating basket/paddle and not less than 10 mm from wall of the vessel. Filter the solution with 0.45 µm porosity filter. Take the absorbance of 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 COA of current lot of prednisone tablet.

ATTACHMENTS

Attachment-I - Calibration Record of Dissolution Test Apparatus (Physical Verification) 
Attachment-II - Calibration Record for Dissolution Test Apparatus (Performance Verification Test) 

REVISION HISTORY 

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