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

2.1  Basket
Stirring Element (USP Apparatus I)

 

 

 

2.2      Paddle
Stirring Element (USP Apparatus II)

 

 

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.

 

 

 

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.

• 5      Acceptance
  criteria: USP allows a tolerance of ± 4 % on the specified RPM.

 

8      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.)