Calibration of Dissolution Test Apparatus
Calibration of Dissolution Test Apparatus
1 MATERIALS REQUIRED
- Instrument under calibration (Dissolution Test Apparatus)
- Monobasic Potassium phosphate
- Water
- Sodium Chloride
- Salicylic Acid Tablets (Non Disintegrating Type)
- Salicylic Acid Standard
- Methanol
- Prednisone Tablets (Disintegrating Type)
- Prednisone Standard
- Calibrated stop watch
- Calibrated Thermometer
- Whatman Filter Paper
- Calibrated Glassware
- Calibrated Tachometer
- Calibrated Vernier calipers
- Approved Kit
2 VERIFICATION OF STANDARD ACCESSORIES
- Basket Stirring Element (USP Apparatus I)
|
Dimension |
Dim |
Dim |
Dim |
Dim |
Dim |
Dim |
Dim |
Dim |
Dim |
|
USP Limits (For |
6.3-6.5 OR 9.4-10.1 |
25.0 ± 3.0 |
20.2 ± 1.0 |
37.0 ± 3.0 |
27.0 ± 1.0 Open Screen |
2.0 ± 0.5 Vent Hole Dia. |
5.1 ± 0.5 |
20.2 ± 0.1 |
22.2 ± 1.0 |
2.2 Paddle Stirring Element (USP Apparatus II)
|
Dimension |
Dim |
Dim |
Dim |
Dim |
Dim |
|
USP Limits (For Paddle1-8) |
9.4-10.1 Before Coating |
42.0 |
74.0-75.0 |
19.0 ± 0.5 |
4.0 ± 1.0 |
2.3 Dissolution Test Vessel
|
Dimension |
Dim A (mm) |
Dim B (mm) |
|
USP Limits (For Jars 1-8) |
160.0-210.0 |
98.0-106.0 |
3 VALIDATION OF PHYSICAL PARAMETERS (USP)
- Basket Wobble
- Paddle Wobble
- Paddle Centering
- D1 MM: D1 is the distance between the bottom edge of the basket to the lowest inner surface of the vessel.
- D2 MM: D2 is the distance between the bottom edge of the paddle to the lowest inner surface of the vessel.
|
Test Position |
Basket |
Paddle |
Paddle |
D1 |
D2 |
|
USP Limits |
± 1 mm |
0.5 mm (proposed) |
Not more than 2.0 mm |
25.0 ± 2.0 mm |
25.0 ± 2.0 mm |
4 CALIBRATION OF THE DISSOLUTION TEST APPARATUS USING SALICYLIC ACID TABLETS (NON DISINTEGRATING TYPE)
USP TYPE I
Dissolution medium : 0.05 M Phosphate buffer, pH 7.40 ± 0.05
Duration : 30 minutes
Temperature : 37°C ± 0.5°C
- Add 2000 ml of phosphate buffer and 1564 ml of 0.2M NaOH and make to 8000 ml with water and adjust the pH to 7.4 ± 0.05.
STANDARD PREPARATION:
- Salicylic Acid standard was previously dried over silica gel, for 3 hours & is dissolved in methanol and diluted with the dissolution medium.
- Further dilute it if required accordingly to the labeled claim of the tablet with dissolution medium.
SAMPLE PREPARATION:
- One tablet is placed in each of the baskets. At the end of 30 minutes withdraw about 20 ml of aliquot and filter through Whatman filter paper no. 41. Reject first few ml of the filtrate. Further dilute the filtrate with the dissolution medium.
- Record the absorbance of the standard and sample solutions at 296 nm using dissolution medium as the blank.
Acceptance criteria: 100 RPM- % release = 23-29
USP TYPE II
- Maintain the same conditions as given under USP TYPE I except that paddles are used instead of baskets. Repeat the procedure as in USP TYPE I and note the absorbance at 296 nm.
Acceptance criteria: 100 RPM- % release = 17-26
5 Calibration of the Dissolution Test Apparatus using Prednisone tablets 10 mg (Disintegrating Type)
USP TYPE I
Dissolution medium : 500 ml Purified water filtered and degassed
Duration : 30 minutes
Temperature : 37°C ± 0.5°C
Volume : 500 ml
Speed : 50 RPM
STANDARD PREPARATION:
- Prednisone working standard was previously dried over silica gel, for 3 hours & is dissolved in methanol and diluted with the dissolution medium.
- Further dilute it if required accordingly to the labeled claim of the tablet with dissolution medium.
SAMPLE PREPARATION:
- One tablet is placed in each of the baskets. At the end of 30 minutes withdraw about 10 ml of aliquot and filter through Whatman filter paper no. 41. Reject first few ml of the filtrate. Further dilute the filtrate with the dissolution medium.
- Record the absorbance of the standard and sample solutions at 242 nm using dissolution medium as the blank.
Acceptance criteria: 50 RPM- % release = 45-75
USP TYPE II
- Maintain the same conditions as given under USP TYPE I except that paddles are used instead of baskets. Repeat the procedure as in USP TYPE I and note the absorbance at 242 nm.
Acceptance criteria: 50 RPM- % release = 35-65
6 LIFT MOVEMENT CHECK
- Lift the unit UP, by pressing the UP key from the front panel. Check for the indicator glow on the UP key and for the smooth movement.
- Take the unit down, pressing the DOWN key from the front panel. Check for the indicator glow on the DOWN key and for the smooth movement.
- Stop the lift in between.
- Fix the Paddle/Basket Rods and check for snap fit.
- Start the stirrer when the lift movement is ON. Stirrer should not Start.
- Repeat the Lift Movement Check procedure for about 3-4 times to ensure the smooth operation.
7. RPM CHECK
- Check the range setting from 25 to 200 RPM attaching all the Paddles/Baskets.
- Set the RPM to 30 and start the instrument and measure the speed of the Paddle/Basket Rod in the test vessel 1-8 using Tachometer. Verify the counts with the set points at 50, 100, 150 & 200 rpm respectively.
- Take at least three to four readings at each set point for better accuracy and reproducibility.
- Correlate the actual readings observed with the set point RPM and apply corrections, if necessary.
- Acceptance criteria: USP allows a tolerance of ± 4 % on the specified RPM.
8 TEMPERATURE CHECK
- Check the range setting from 30°C to 40°C Temperature.
- Fill the jars with water and place them in the bath.
- Check the temperature at the following condition.
- Check the temperature inside the bath with the traceable thermometer with 0.1°C resolution.
- Verify the measured bath temperature with the displayed bath temperature.
- Now set the temperature to 37.7°C (for Merion Jars). Switch the heater by pressing TEMP Key and F1 key resp.
- Wait till the temperature reaches the set value. The READY indicator will glow.
- Verify the temperature in bath with the standard calibrated thermometer.
- Wait till the temperature in the individual test vessels reaches to 37.0°C and record the readings in the test vessel 1-8.
9 RUN TEST
- Check for the READY indicator on the front panel.
- Check for the printer connection (if Attached) and make sure the printer is switched ON. Load the paper in the printer and leave the printer in READY condition.
- Set the Test Parameter as required. Start the test pressing the START key. Check for the RUN indicator on the front panel.
- Check the Timer with the standard calibrated stop-watch.
- After the set print Interval Time, the test results will be printed. Check the tests print outs.
10 . TUBE CALIBRATION AND SAMPLE TIME CALIBRATION (IN CASE OF AUTO SAMPLER)
- Let Power ON and check for peristaltic Pump and Fraction Collector.
- Check the direction for the Peristaltic Pump.
- Let the Arm Forward and Reverse Check for the Fraction Collector.
- Set the parameter for replenishment to ‘yes’.
- Perform the tube calibration (TC) procedure and sampling time (ST) procedure for the sample volume of 10 ml.
- Note the Tube time reading displayed and sampling time reading displayed for 1 ml using stop watch.
- Repeat the above procedure for 1 more monograph and different sample volume and note the time reading displayed for 10 ml.
- Check time taken for reverse run using stop watch.
- Compare (TC + SC) with reverse run time.
- Take 6 readings for both sample volumes and replenishment volumes measured in ml for 5 and 10 ml.
11 CALIBRATION FREQUENCY
Physical – At every 3 months
Chemical – At every 6 months (Prednisone Tab.)
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