Operation and calibration of dissolution test apparatus

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Operation and calibration of dissolution test apparatus

1.0 Purpose
1.1 To describe a procedure for operation and calibration of Apparatus.

2.0 Scope
2.1 This standard operating procedure is applicable for operation and calibration of Dissolution

Test Apparatus located at Instrument Room in Quality Control Laboratory at ABC Pvt. Ltd.

3.0 Responsibility
Officer QC/ Executive QC Preparation of SOP and follow the procedure as per SOP
Assistant Manager Reviewing and Training of SOP
Manager QC Implementation of SOP
4.0 Accountability
4.1 Manager Quality Control is accountable for implementation and compliance with SOP.

5.0 Procedure
5.1 Operation
5.1.1 Connect the system with main power supply and the heater plug in the

socket provided at the rear panel of the stirrer unit.
5.1.2 Check the water level of the tank, and make up to the mark, if required.
5.1.3 Switch ON the power switch provided on the left side of back panel of stirrer unit.
5.1.4 Put the jars in tank.
5.1.5 Switch ON the heater switch provided on the left, side of back panel of stirrer unit of the instrument.
5.1.6 Set the program on the instrument as follows.
5.1.7 Set the program on the in Press the STEP/PROGRAM key. The SET STEP key

led will be ON, then press required step in the desired range of (0-13). Enter number 1 key

and then press ENTER key to acknowledge the data, this in turn shall make the set STEP/PROGRAM key OFF.
5.1.8 Press the SET/TIMER key to set the time. The LED on the key shall be ON.
5.1.9 Enter the required time for setting Hour & minute from the keypad. Press ENTER key

to acknowledge the data. This in turn will make LED OFF.
5.1.10 Press the SET/RPM key to set the RPM. The LED on the key shall be ON.
5.1.11 Enter the required RPM value from the number keypad and then press ENTER key to

acknowledge the data. This is turn will make the LED of the SET/RPM key OFF.
5.1.12 Press the SET/TEMP key. The SET TEMP key LED will be ON.
5.1.13 Set the temperature to 37 °C, unless otherwise specified, from the number keypad.

Press ENTER key to acknowledge the data. This in turn will make the LED of SET/TEMP key OFF.
5.1.14 Press START/STOP TEMP. Key to start the temperature to the desired value.
Note: Check the temperature indicator is ON. To view the set temperature presses

the SET/TEMP key again.The temperature display unit will now show the

temperature on the screen.
5.1.15 Lift the stirrer unit using up key.
5.1.16 Place the dissolution jars into the water bath in their fixed slots.
5.1.17 Fix the shaft with paddle/ basket (Apparatus I or II as per requirement)

on stirrer unit carefully & tighten them.
5.1.18 Prepare the dissolution media as per the standard test procedure and

fill the jars with the medium.
5.1.19 Bring the stirrer unit down using the down key (provided on right hand

side of the front panel). The stirrer unit shall automatically stop at the required height.
5.1.20 Keep the stirrer to stay in the medium till medium in the jar attains required temp.

Check the temperature of the jars with calibrated thermometer.
5.1.21 Wait to achieve the set temperature. This shall be indicated by blow of READY indicator.
5.1.22 After attaining the READY status, place the tablets in each jar (in case of paddle)

or in basket as per the STPs requirement. In case basket is used, the stirrer unit is put

up by putting the lift up/down switch to up position, stopping the stirring and fixing

the basket with sample on the shaft. Again switch on the stirring and bring the stirrer

unit down by putting the left up/down switch to down position.
5.1.23 Press the START TEST key immediately to start the timer and stirrer.
5.1.24 Wait to complete the dissolution time. It will give a beep sound.
5.1.25 Press STOP STIRRER, the instrument will stop automatically.
5.1.26 Withdraw the sample from a zone midway between the surface of the dissolution

medium and top of the rotating basket or blade, not less than 1 cm from the vessel wall.
5.1.27 Put the stirrer unit up by switch to up position.
5.1.28 Switch OFF the heater and main power supplies switch.
5.1.29 Remove the dissolution medium from the jars and wash with water till the jars are

free from traces of dissolution medium solution.
5.1.30 Remove the jars, discard the medium and clean the jar.
5.1.31 Unscrew the Paddle / Basket and clean with the distilled water and wipe with

tissue paper and preserve at designated place.

5.2 Calibration
5.2.1 Calibration of Physical Parameters (Quarterly)
5.2.2 Calibration of Chemical Parameters (yearly)
5.2.3 Operate the instrument as per procedure given above procedure.

5.3 Calibration of Physical Parameters (Quarterly)
5.3.1 Head Co-planarity (Base leveling)
5.3.1.1 A spirit level should be used to ensure that both the head plate and the

base plate are perfectly horizontal.\
5.3.1.2 A spirit level should be kept on the head plate to check that the head

plate is perfectly horizontal.
5.3.1.3 If it is not horizontal, the bath should be removed and the base plate under the

bath should be checked with the spirit level.
5.3.1.4 A base plate should be brought to the planarity and then the bath should be

kept in its place and the head plate should be checked for the planarity.
5.3.1.5 Acceptance criteria: The apparatus should be in level

5.3.2 RPM (Revolution per Minute)
5.3.2.1 Make instrument ready for analysis with paddle at 50 RPM.
5.3.2.2 Place the magnetic clip on the paddle or basket shaft being checked. To avoid

damage to the paddle or basket shaft, place the clip on the near to top of the shaft, just

below the spindle chuck, then slide it down into its operation position in front of th

e tachometer sensor and Record the RPM.
5.3.2.3 Follow the same procedure for remaining vessels.
5.3.2.4 Repeat the same procedure at 100 RPM.
5.3.2.5 Acceptance criteria: Set the value ± 4%
5.3.3 Temperature
5.3.3.1 When set temperature is attained, check the temperature of the individual vessels

by using the calibrated thermometer and record the temperature.
5.3.3.2 Follow the same procedure for remaining vessels.
5.3.3.3 Acceptance criteria: 37oC ± 0.5oC
5.3.4 Jar centering
5.3.4.1 Make instrument ready for analysis.
5.3.4.2 Loose the base plate of each vessel, fix the centering device with spindle, lower

down the spindle inside the vessel (the jar is automatically centered) and tighten the base plate of each vessel.
5.3.4.3 Fix the wobbling gauge in each vessel, rotate by 360° and record the reading.
5.3.4.4 Follow the same procedure for remaining vessels.
5.3.4.5 Acceptance criteria: Each jar: NMT 2 mm on 360° revolution

5.3.5 Shaft wobbling
5.3.5.1 Make the instrument ready for analysis by setting the shaft speed at 50 RPM.
5.3.5.2 Attach the wobbling meter to the shaft whose wobbling is to be measured. Press

and hold briefly ORIGIN to auto zero the gauge. The screen display 0.00 mm.
5.3.5.3 Ensure the wobble gauge is properly positioned with the tip of the wobble gauge pointer

positioned against the paddle shaft or the bottom rim of the basket.
5.3.5.4 Record the shaft wobbling. Repeat the procedure for remaining shafts.
5.3.5.5 Acceptance criteria: Basket NMT 1 mm & Paddle NMT 0.5 mm

5.3.6 Time displayed
5.3.6.1 Set the time in instrument to 30 minutes. Start the equipment & stopwatch simultaneously.
5.3.6.2 Note down the time on the stopwatch when the set time is off displayed by equipment.
5.3.6.3 Repeat the procedure for 45 minutes and 60 minutes.
5.3.6.4 Acceptance criteria: ( 1 minute of stated time)

5.3.7 Paddle / Basket Depth
5.3.7.1 Use calibrated vernier.
5.3.7.2 Keep all jars empty and remove lid from it.
5.3.7.3 Lower the stirrer unit to the bottom position till it stops automatically.
5.3.7.4 Use the above vernier, hold it vertical and touching parallel to the paddle shaft.
5.3.7.5 Touch the reference bracket of the vernier at bottom face of paddle.
5.3.7.6 Slide vernier scale down till the point of stylus touches the jar bottom.
5.3.7.7 Lock the vernier at this position and lift up the stirrer unit.
5.3.7.8 Repeat the same procedure for remaining vessels. Record the result in calibration format.
5.3.7.9 Acceptance criteria: The distance should be 25.0 ± 2.0 mm.

5.4 Calibration of Chemical Parameters (yearly)
5.4.1 Prepare the dissolution media as per procedure given in Annexure II
5.4.1.1 Standard preparation
5.4.1.1.1 Weigh about 60 mg of Prednisone USP reference standard in 200 ml volumetric flask,

add 10.0 ml ethanol to dissolve and make the volume with purified water. Further dilute 5 ml

of above solution to 100 ml with purified water for apparatus 1 (Basket) and Further

dilute 5 ml of above solution to 200 ml with purified water for apparatus 2 (Paddle).
5.4.1.2 Sample preparation
5.4.1.2.1 Tablet 500ml of purified water
5.4.1.2.2 Apparatus : Type-1 (Basket) & Type-2 (Paddle)
5.4.1.2.3 Medium : 500 ml water
5.4.1.2.4 Medium Temp.: 37°±0.5°C
5.4.1.2.5 Time : 30 Minutes
5.4.1.2.6 RPM : 50 RPM
5.4.1.2.7 Wavelength : 242 nm
5.4.1.3 Ensure the lot No. of tablet is current.
5.4.1.4 Place one tablet in each jar after instrument get ready and start the instruments.
5.4.1.5 After the set time will over there will be long beep and the instruments will stop automatically.
5.4.1.6 Filter the solution and measure the absorbance on the UV at 242 nm.

For standard and sample simultaneously and calculate the % dissolve and record.
5.4.1.7 Acceptance Criteria: As per current tablet lot Number’s COA.

5.5 Cleaning and Precaution
5.5.1 Disconnect the Instrument from main power supply
5.5.2 Clean the instrument externally with clean dry cloth daily.
5.5.3 Clean the dissolution bowls after every dissolution test.
5.5.4 Remove the water from tank twice a month and clean with wet cloth soaked in hot water.

After due cleaning of the tank, fill the tank with water. Also clean externally with a wet cloth.
5.5.5 Report any discrepancy observed during operation of the instrument to Manager-QC or

his authorized representative, and notify the defect to Engineering

Department/ Service Engineer to rectify the defect. Affix ‘Under Maintenance’ label on the instrument.

6.0 Reference
Indian Pharmacopoeia/USP/In-house

7.0 Attachments
Annexure I: Calibration Record of Dissolution test apparatus (Physical Parameter)
Annexure II: Calibration Record of Dissolution test apparatus (Chemical Parameters)

8.0 Distribution
Distribution of the controlled copy to concerned departments.
Additional copies may be issued for specific purpose.

9.0 Abbreviations
QA : Quality Assurance
QC : Quality Control
SOP : Standard Operating Procedure
RPM : Revolution Per Minutes

10.0 Revision History