Operation and Calibration of Dissolution Test Apparatus

Purpose

This SOP describes the procedure for Operation and Calibration of Dissolution test apparatus.

Procedure :

Operation  

• Switch ‘ON’ the Main.
• Switch ‘ON’ the instrument by pressing the “Power” and “Heater ON” buttons of  Temperature Controller .
• After the power flash screen, an Idle screen shall be displayed showing Electrolab (Make)Dissolution Apparatus Model- EDT 08 Lx VER-4.51 ELABDISSO
• Then Display show Date, RPM, BATH, EXT,  PROTOCOL. MENU and PREPARE.
• Go to Menu to select RPM, Time and Temperature as per Standard Testing Procedure (As given below in 4.2 Protocol setting) Then load Protocol which was given in Edit Protocol.
• After settings of Protocol Press <Start> Key of system.
• Place the test vessels filled with the media, in such a way that  the jar clamp are setle in the groove of the jar provided at jar flange, and rotate the jar clockwise or anti- clockwise

Protocol Setting

• Go To Menu on the Screen to Prepare the Protocol. Press F1 from the Front panel.
• Then 7 options will show on the screen- 1. Configure   2. Protocol   3. Settings      4. Reports 5. Run 6. Jar Temp 7. Version
• Press 2 from Alphanumeric Keypad to Enter Protocol Menu.
• Then Three Options will Show on the screen-
•  1. Load Protocol
•  2. Edit Protocol
•  3. View Protocol.
• Press 2 to Enter Edit Protocol. Select the Desired Protocol which needs to Edited using Up/ Down arrow and Press Enter Key.
• Enter the Parameters in Protocol Such as DRUG NAME: (Press F3 from Front     Panel to   Save and go to the Next parameter)
• MEDIA NAME: (Press F3 from Front Panel to Save and go to the Next parameter)
• pH VALUE: <00.0 - 14.0>: (Press F3 from Front Panel to Save and go to the Next         parameter)
• TEMPERATURE:  °C <20.0– 40.0>:(Press F3 from Front Panel to Save and go to       the Next parameter)
• MEDIA VOL:   ml <0050 - 1000>: (Press F3 from Front Panel to Save and go to the     Next parameter)
• POWER FAIL: Min <01-40>: (Press F3 from Front Panel to Save and go to the Next     parameter).
• APPARATUS: Press Enter Key then 6 options will show on the screen 1. Basket 2.        
• Paddle 3. Paddle+ Disk 4.Trans1 5.Trans2 6.Paddle45. In Apparatus Parameter select desired apparatus by using alphanumeric key (Press F3 from Front Panel    to Save and go to the Next parameter)
• Time Table: Press Enter Key and submit the Sampling time intervals by using alphanumeric key & press arrow key to go RPM.
• RPM: <20 to 250> Select by using alphanumeric keys. Press arrow key.
• Total: no of samples <1 to 24> select by using alphanumeric keys as per Standard Testing Procedure.
• Now Press F3 From Front panel to ‘’Save & Back’’ and again Press F3 for ‘’Save & Exit’’
• Protocol can be view before Start the system. Press 3 in the Protocol to View Protocol.
• Press 1 to Enter Load Protocol; Enter the no of Edited Protocol on the Screen by pressing arrow key, Press Enter. The massage “Proto. Loaded” appear then Press “Esc” Key to escape out.
• After Load Protocol ‘Prepare’ show on the screen. Press F2 and Enter Batch No., A.R. No. of the Sample.
• “Press UP to Edit or Press Enter to Proceed” will Show on the Screen Display. Press Enter.
• After attaining the Temperature, the screen will Show “Drop Tablet & Press Start” and the LED light of Ready will glow on the front Panel.
• Press START key for starting the operation. After pressing START the LED light of RUN will glow on the front Panel.

RPM Setting

Set the RPM by pressing RPM key provided on front panel, the screen shall display as-

SET RPM: 250 (20 - 250) Motor is Stopped                  

Temperature Setting

• Press TEMP key on front panel to set the desired temperature for Test and to Start the Temperature controller, the screen shall display as-
• SET TEMP: 37.5⁰ C                       (20.0 – 40.0⁰ C)
• Press F1 Key to Turn on the Temperature, F2 for pump on and F3 to Turn off the    Temperature.
• Then Press “Esc” Key to escape out.
• In the condition of ON Temperature controller, The LED light of Temperature will glow on the front panel. If heater is ON, then BATH & EXT probe on the screen will show the rise in temperature simultaneously till attain the set Temperature.
• If Heater is in OFF condition, on the screen, BATH & EXT probes will display the Room temp. or surrounding temperature.

Gradient Temperature

Gradient temperature is the difference in temperatures of BATH and JAR.Press F1 Key From front panel to enter Menu Screen. Then Press 1 from alphanumeric keypad to enter “Configure”. Then Press 3 to Enter Temp Grad. Set Temp Gradient up to 1.5⁰ C Using Arrow Key.

Gradient Temp: 0.7⁰ C ˄˅

Temp control ON after test over?

ON                                        <OFF>                                     SAVE

Press F1 key to on the Temperature Controller.

Press F2 key To OFF the Temperature Controller

Press F3 key To “SAVE”

Then Press “Esc” Key to escape out.

Power Failure During Operation

Go To Menu on the Screen. Press F1 from the Front panel.

Then 7 options will show on the screen- 1. Configure   2. Protocol   3. Settings      4. Reports 5. Run 6. Jar Temp 7. Version

Press 2 from Alphanumeric Keypad to Enter Protocol Menu.

Then Three Options will Show on the screen-

          1. Load Protocol

          2. Edit Protocol

          3. View Protocol

Press 2 to Enter Edit Protocol. Select the Desired Protocol which needs to Edited using Up/ Down arrow and Press Enter Key. Press F1 key again & again till the option of Power Fail will appear on the screen.

POWER FAIL: In Power fail enter the time from 1-40 minutes. If power is resumed back within set time the test will start automatically. Press F3 to Save from Front Panel.

Then Press “Esc” Key to escape out.

System Settings

Go To Menu on the Screen. Press F1 from the Front panel.

Then 7 options will show on the screen- 1. Configure   2. Protocol   3. Settings      4. Reports 5. Run 6. Jar Temp 7. Version

Press 3 to Enter Settings. Then 3 options will show on the screen-

Clock

Wakeup

Security

Clock:

Press 1 from Alphanumeric Keypad to Enter “Clock”.

Set Date and Time using ˄˅ < ˃ Arrow keys.

Press F1 from front panel to save the entered date and time, the Idle screen         will be displayed.

Press F3 from front panel to go back to the setting screen.

Wakeup:

In this parameter the sleep mode time and date are set. The instrument will           start automatically at set time and date for the bath temperature to attain.

Press 2 from setting screen.

Wake up time and date needs to be added using Up/Down & Side arrow    keys.

Press F1 key ON the Wake up Parameter, the LCD Display light will be off automatically & Idle screen will be displayed.

Security:

Press 3 to enter Security Menu.

This is done by issuing username and Password.

To Enable: Press 1 to enable security, Username and password needs to be        added.

Press F1, Access granted screen will be flashed & Idle screen will be          displayed.

To Disable: Press 2 For Security Menu.

Idle Screen will be displayed Security option.

Calibration of Physical Parameters (Frequency: Quarterly)

                        Level Adjustment

                        Basket Integrity

                        Jar Centering

                        Timer

                        Spindle speed (RPM)

                        Shaft Paddle / Basket wobble test

                        Paddle / Basket Depth

                        Vessel Temperature (ºC)

Level Adjustment

Before going to calibrate ensure the level of dissolution test apparatus.

Adjust the level by rotating the wheel provided in the bottom.

Check the instrument level using Spirit Level.

Basket Integrity

Check the basket sieve for any damage before calibration.

Jar Centering

Loose the base plate of each jar, fix the centering device with spindle, lower down the spindle inside the jar (the jar is automatically centered) and tighten the base plate of each jar.

Fix the wobbling gauge in each jar, rotate by 360° C and record the reading.

Timer

Set the time in instrument to 30 minutes. Start the equipment & stopwatch simultaneously.

Note down the time on the stopwatch when the set time is off displayed by equipment.

Spindle Speed

Set the RPM of the instrument to 50 and 100 alternatively. Bring the tachometer in contact with each spindle, start the revolution and record the reading. Else attach a paper flag on each spindle and start the revolution and count the number of revolutions per minutes visually.

Document the activity in Calibration Record of Dissolution Test Apparatus.

Shaft (Paddle / Basket) Wobble Test

Ensure that shaft of Basket/Paddle is clean and free from any particle.

Paddles/ Baskets are firmly tight to the main spindle.

Position the Wobbling gauge in each Jar approximately 2. mm above the Paddle/Basket unit in such a way that the apparatus does not touch the Paddle/ Basket.

Set RPM of the instrument to 50. Operate the instrument and measure the Wobbling of each shaft and basket in mm.

Document the activity in Calibration Record of Dissolution Test Apparatus

Paddle / Basket Depth

Fix the paddle and basket in each spindle alternatively.  Measure the distance between the bottom edge of paddle blade / basket to the lowest inner surface of the jar with the help of Depth gauge. Document the activity in Calibration Record of Dissolution Test Apparatus.

Vessels Temperature

Place the vessels in the constant temperature water bath, and allow the dissolution medium to come to a temperature at 37^oC ± 0.5^oC.

The temperature of the purified water must be at 37^oC ± 0.5^oC before the tablets are immersed, and this temperature must be maintained throughout the

procedure.

Ensure the temperature of vessels within range using calibrated thermometer.

Document the activity in Calibration Record of Dissolution Test Apparatus

Acceptance criteria for physical parameters

Parameter	Acceptance Criteria
Level adjustment	Spirit level should be in  middle
Basket integrity	Basket sieve should be free from any damage
Jar Centering	Each jar: NMT 2 mm on 360° revolution
Timer	29 to 31 Minute
Spindle Speed: 50 RPM 100 RPM	48 to 52 RPM 96 to 104 RPM
Shaft (Paddle/basket) Wobble	NMT 1 mm
Paddle/Basket Depth	23 to 27 mm
Vessel Temperature	37°C ± 0.5°C

           *Reference USP / In-House

SYSTEM SUITABILITY: (Frequency: Half Yearly)

Perform dissolution performance verification test using USP Prednisone RS tablets (Disintegrating Type Tablet).

Carry out the procedure using USP TYPE-I (basket) and TYPE-II (paddle) Dissolution Test Apparatus maintaining following parameters.

                        Medium                     : De-aerated purified water

                        Volume                       : 500 ml

                        R.P.M                         : 50

                        Temperature             : 37^oC ± 0.5^oC

                        Time                          : 30 minutes

Standard Preparation:

Accurately weigh about 20 mg of Prednisone USP RS in 100 ml volumetric flask.

Add not more than 5 ml of alcohol to dissolve.

Make up the volume with de-aerated purified water.

Further dilute 5 ml of this solution to 50 ml with de-aerated purified water.

Method for de-aeration:

Heat the purified water while stirring gently to about 41^oC then cooling to 37^oC before use.

Immediately filter under vacuum using a filter having porosity of 0.45 µm.

Dissolution Procedure:

Set the parameters of the instruments as mentioned above.

De-aerates the medium prior to use.

Place 1 tablet in each of six different vessels containing 500 ml of purified water.

Operate the apparatus for exactly 30 min.

At the end of 30 min withdraw the solution from zone midway between the surfaces of the medium and top the rotating          paddle not less than 1 cm from the vessel wall.

Immediately filter the solution through 0.45 µm.

Discarding first few ml of the filtrate.

Measure the absorbance of the standard preparation and sample preparation by UV Spectrophotometer at maximum 242 nm against water as blank.

Calculate the percentage of Prednisone dissolve in 30 minutes in     individual tablet using following formula.

                            Standard weight          5            500

             Factor = ------------------------x---------x-----------x Std. Potency

                                       100                   50         Claim

                                                   Test absorbance

% of Prednisone dissolved = ------------------------------ x Factor

                                                            Standard absorbance

                        

Document the activity in Calibration

Action During Out of Calibration:

Report any discrepancy observed during calibration of instrument to Analytical Development Laboratory In-Charge or his designee for corrective and preventive action.

Analytical Development Laboratory In-Charge or his designee           informs the defect to Maintenance Department service engineer to    rectify the defect. Affix ‘Under Maintenance’ label on the instrument.

Calibration should be required after maintenance.

Precautions

Don’t expose the tablets to excessive humidity.

Store the tablets at 15^o to 25^oC.

Cleaning procedure         

Cleaning procedure for Apparatus

(Frequency: After completion of every dissolution test)

Lift the stirrer unit by pressing UP key.

Switch off the heater.

Switch off the instrument.

Switch off the main.

Remove the basket/paddle apparatus from the dissolution tester. Wash them with tap water, then with 0.5% teepol solution, finally with purified water, dry with tissue paper and keep at proper place.

Remove the bowls and discard the medium of each bowl. Wash each bowl properly with tap water after, then with 0.5% teepol solution, finally with purified water and keep them inside the dissolution bath serial wise.

Keep the record in instrument usage logbook.

Cleaning procedure for water bath.

• (Frequency: Once in a week or before if necessary)
• Lift the stirrer unit by pressing UP key.
• Switch off the heater.
• Switch off the instrument.
• Switch off the main.
• Remove the basket/paddle apparatus from the dissolution tester.
• Remove all the bowls from the water bath.
• To drain the used water, a pipe containing tap at the end of pipe is attached just under the water bath.
• Open the tap and drain the used water in a waste bucket.
• Remove the circulating pipes and clean internally with long brushes.
• Wash the water bath with tap water, then with 0.5% teepol solution and after that again with tap water, until no any foam remain in the bath. After complete removal of the teepol solution, wash the bath finally with Purified water.
• Fill the bath with Purified water up to level mark.