SOP for Operating the Tablet Dissolution Apparatus

1.0   Objective

The objective of this Standard Operating Procedure is to lay down the procedure for operating the Tablet Dissolution Apparatus 

2.0       Scope

This SOP covers operating procedure of Tablet Dissolution Apparatus 

3.0       Responsibility

Jr. Research Officer, Research Officer: Responsible for operation, calibration and maintenance of the instrument as per procedure.

Head of Department: Responsible for calibration and maintenance, timely as per schedule.

QA Officer/QA Manager: Review the records and governing the document.

4.0       Procedure

4.1       Ensure the instrument is Clean & Free from Dust

4.2       System Start Up

4.2.1    Switch ON The ETC-11L instrument by pressing the power button

4.2.2    Now, Switch ON the Power switch provided on rear side of TDST-08L the instrument will initialize by displaying a power flash screen, which will flash once.

4.2.3    After the power flash screen will be displayed showing the last protocol no selected, RPM, Bath temperature, and temp by external probe.

4.2.4    Raise the instrument by pressing the lift UP Key provided in the front panel TDT-08L.

4.2.5    Remove the bath Top Plate and fill the bath with R.O or distilled water till the bottom of the inlet Nozzle. Once the tube of the inlet nozzle is filled with water, ensure the priming of the pump. Then fill water till the level marked. Place the bath top plate and tighten the

plate retaining Knob

4.2.6    Place the test vessels filled with the media.

4.2.7    If required check the centering of the Test Vessel.

4.2.8    Set the test parameter as desired.

4.2.9    Parameter Setting:

RPM Setting:

In this parameter rotation per minute of the shaft are set from 25 to 200 RPM

Setting Of spindle RPM Press RPM key from front panel a RPM screen will be displayed than set the RPM by pressing UP/Down/Digit scroll key and enter to register the value. Than come out the RPM mode.

For starting and stopping of spindle rotation Press RPM key and than F1 for starting and F2 for Stopping

Temperature Setting:

In this parameter temperature of the bath is set from 30°C to 40°C

Press the TEMP key from the front panel a Temperature screen will be display than set the Temperature by using UP/Down/Digit scroll key and enter key to register the value. Than come out the Temperature mode. 

For Heater ON/OFF Press TEMP key and than F1 for Heater to be ON and F2 for Heater to be OFF.

Indication

If the temperature controller has started then the ONLED on the front panel and ETC-11L will glow.

If HEATER ON then the circulating pump will start by default

Run Time

To set the run time press TIME key from the front panel and set the time by pressing UP/Down/ Digit Scroll key and enter key to register the value. Than come out the time mode 

4.2.10  Lower the stirrer unit by pressing the down arrow key from the front panel. 

Press F1 Key (PREPARE) for starting of test, the temperature controller will be on.

4.2.11  To attain a constant temperature through out The vessel start the RPM with paddle attached to the spindle.

4.2.12  After getting the desired temperature at the lowest position of the stirrer unit (as per the method selected) the ready indication on the front panel will glow.

4.2.13  To View the individual jar temperature in between the test or prior to the test, from idle screen press F2 key to select jar probe.

Caution: If F1 key pressed to start the test and stirrer unit is not at the lowest position then an error indication will be display for 5 sec, Press down arrow key to park the stirrer unit at lowest position and rectify the error indicated.

4.2.14  To start the testing lift the stirrer unit and place the test sample in basket if using apparatus 1 and in jar if using apparatus2 than down the stirrer unit by pressing down key and start the test. 

5.0       Calibration:

5.1       CALIBRATION OF TEMPERATURE:

5.1.1    Set 37˚ C and measure the temperature using calibrated thermometer.

5.1.2    Of inside vessel at the following intervals : 30 minutes, 45 minutes, 1 hour, 2 hours, 4 hours.

5.1.3    Limit : The observed value should be between 36.5˚ C to 37.5˚ C.

5.1.4    Record the observations as given in the Annexure - 2.

5.2       CALIBRATION OF SPEED:

5.2.1    Set the speed as 50 RPM and measure the number rotations at the following time   intervals :  30 minutes, 45 minutes, 1 hour, 2 hours, 4 hours.

5.2.2    Limit: ± 4 % of the set speed.

5.2.3    Record the observations as given in the Annexure - 2.

5.2.4    In the same way, set the speed as 100 RPM and measure the number rotations at the following time intervals: 30 minutes, 45 minutes, 1 hour, 2 hours, 4 hours.

5.2.5    Limit: ± 4 % of the set speed.

   5.2.6    Record the observations as given in the Annexure - 2.

5.3       WOBBLING :

5.3.1    Check the shaft paddle wobbling using wobble meter at different time intervals as follows: 30 minutes, 45 minutes, 1 hour, 2 hours, 4 hours.  (Limit : ± 2 mm from vertical axis) Record the observations as given in the Annexure - 2.

5.3.2    Check the basket wobbling using wobble meter at the following time intervals as  follows: 30 minutes, 45 minutes, 1 hour, 2 hours, 4 hours.   (Limit : ± 2 mm of maximum allowable run out at the bottom).

5.3.3    Record the observations as given in the Annexure - 2.

5.4       DISTANCE BETWEEN THE BOTTOM OF THE VESSEL AND THE BASKET:

5.4.1    Measure the distance between the bottom of the vessel and the basket. Limit: 25 ± 2 mm.

5.4.2    Record the observations.

5.5       CENTERING OF DISSOLUTION VESSEL:

5.5.1    Using the centering device check whether the dissolution vessel is at center.

5.5.2    If it is not at the center, then adjust its position to the center.

5.6       Calibration Frequency: Monthly for above parameter

5.7       Calibration with USP calibrators:

5.7.1    Use the following dissolution calibrators:

 Disintegrating type Prednisone tablets.

Use current lot of the above tablets for calibration.

5.7.2    To be prepared and use dissolution medium as per catalog given with USP calibrators tablets specification from the source.

5.7.3    To set all the parameters e.g. RPM, Apparatus 1 or 2 (Basket or paddle), temperature and time as per given in specification.

5.7.4    After completion of USP calibrator calibration calculate the percentage and compare with Acceptance Criteria as per given in specification.

5.7.5    Enter the details of calibration record in Annexure – 2.

5.8              Calibration Frequency: Yearly for USP calibrator tablet

6.0                    Routine maintenance:

6.1                    Disconnect the instrument from power supply.

6.2                    Remove the water from tank. Clean the water tank with dry cloth and replace the fresh distilled water.

6.3                    Clean the Basket –Paddle and Bowl with water and than dry cloth.

6.4                    Clean the instrument with dry cloth.

7.0       Documentation:

Annexure – 1     Instrument usage log book                                             XXX/FRM/000-00

Annexure – 2     Dissolution Apparatus Calibration Record Format       XXX/FRM/000-00

8.0         History of Revision:

Revision No.	Effective Date	Revision details	Reason for revision

Annexure – 1
Date	A. R. No.	Name of Sample	B. No.	Used by	Remark
SOP No. : XXX/SOP/000                                                                Format No. : XXX/FRM/000-00

Annexure – 2
Physical Parameters Calibration of Dissolution Test Apparatus							Page No. : 01 of 02
Calibration Date   :                                                Next due date for calibration : Make                    :                                                Model No. :
Calibration Parameter	Unit No.	Unit - 1	Unit - 2	Unit - 3	Unit - 4	Unit - 5		Unit - 6
	Time
Temperature Limit :  37.0° ± 0.5° C	30 Minutes
	45 Minutes
	1 Hour
	2 Hour
	4 Hour
Shaft (Paddle) wobbling Limit : ± 2 mm from vertical axis	30 Minutes
	45 Minutes
	1 Hour
	2 Hour
	4 Hour
Basket wobbling Limit : ± 2 mm from vertical axis	30 Minutes
	45 Minutes
	1 Hour
	2 Hour
	4 Hour
Rotation per Minute  Set 50 (Limit : 4 % of set speed)	30 Minutes
	45 Minutes
	1 Hour
	2 Hour
	4 Hour
Rotation per Minute  Set 100 (Limit : 4 % of set speed)	30 Minutes
	45 Minutes
	1 Hour
	2 Hour
	4 Hour
Distance (Limit :  25 ± 2 mm)
Remarks : Satisfactory / Not Satisfactory Calibrated by  :                                                                      Checked by      :
SOP No. : XXX/SOP/080                                                               Format No. : XXX/FRM/000-00

Annexure – 2
Calibration of Dissolution Test Apparatus by USP Calibrators Tablets							Page No.: 02 of 02
Calibration Date   :                                                Next due date for calibration : Make                    :                                                  Model No. :
1.                          1.       CALIBRATION BY DISINTEGRATING TYPE PREDNISONE TABLETS : 1.1     Lot No. : 1.2     Standard Preparation : 1.3     Sample Preparation : 1.4     Dissolution Condition :           Dissolution Medium :           Temperature             :           Speed                        :           Apparatus                 :  (1) Basket or (2) Paddle             Calculation Formula :
Unit No.	Apparatus 1 (Basket)			Apparatus 2 (Paddle)
	Absorbance	mg/Tablet	%	Absorbance	mg/Tablet	%
1
2
3
4
5
6
Acceptance Criteria
Remarks : Satisfactory / Not Satisfactory Calibrated by :                                                                     Checked by :
SOP No. : XXX/SOP/000                                                             Format No. : XXX/FRM/000-00