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

2.1  Basket
Stirring Element (USP Apparatus I)

 

Dimension

Dim
A

(mm)

Dim
B

(mm)

Dim
C (mm)

Dim
D (mm)

Dim
E (mm)

Dim
F (mm)

Dim
G (mm)

Dim
H (mm)

Dim
J (mm)

 

 

USP Limits

(For
Baskets1-8)

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
A (mm)

Dim
B (mm)

Dim
C (mm)

Dim
D (mm)

Dim
G (mm)

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
Wobble

Paddle
Wobble

Paddle
Centering

D1
MM

D2
MM

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.

7RPM 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.)

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