Friday, December 10, 2010

OPERATION AND CALIBRATION OF DISSOLUTION TEST APPARATUS

1.0.            OBJECTIVE: To describe a procedure for the operation and Calibration of dissolution test  apparatus, to ensure that the instrument performs satisfactorily and gives accurate and reproducible data.

2.0.            RESPONSIBILITY:

2.1               The Officer - Quality Control shall be:

2.1.1.        Responsible for operating the Dissolution Apparatus as per the SOP.
2.1.2.        Responsible for timely calibration of Dissolution Apparatus as per the SOP.

2.2               The Executive - Quality Control shall be:

2.2.1          Responsible for ensuring the adherence of SOP.

3.0.            PROCEDURE:

4.1              PROCEDURE FOR GENERAL CLEANING:

Ø                  Ensure that the power supply to the instrument is switched OFF before cleaning.
Ø                  Clean the equipment with a clean dry cloth every day. Occasionally wet cloth dipped in dilute soap solution may be used.
Ø                  Precaution shall be taken to clean the equipment immediately with dry cloth to remove the moisture, Switch on the power switch and heater switch provided on the top.
4.2              OPERATION

Ø                  Switch on the power switch and heater switch provided on the top.
Ø                  When the power is switched on the following menus are displayed
Ø                  The STEP / PROGRAM display shows "sd " & the remaining displays are blinking and indicating that the system is going through "SELF DIAGNOSTICS ".
Ø                  All the displays flash "B.B. -----" twice.
Ø                  Then the system gives a long beep.
Ø                  The step display then defaults to 1, which corresponds to Time Interval  & RPM.
Ø                  Then the bath tank is illuminated and the temperature display shows the bath temperature and set the Temperature 37 ± 1°C.
Ø                  Lift the stirrer unit using the (UP ▲) key.
Ø                  Put the jars filled with the medium in tank.
Ø                  Fix paddle / Basket (as per the respective monograph) screw the same on the spindle carefully and tighten it using the LN keys.
Ø                  Bring the stirrer unit down using (DOWN ▼) key.
Ø                  The stirrer unit will automatically stop at the required height (i.e. Paddle / Basket will be 25 mm above the jar bottom).
Ø                  Start the stirrer by using the (START / STOP) key.
Ø                  Start the temperature by using the (START / STOP) key.
Ø                  Once the set temperature is attain (READY) put the tablets in the test jar or baskets.
Ø                  Cover the jars with the lids.
Ø                  After the completion of specified run time, the machine will give a long beep sound indicating that the test is completed, then proceed the further as per specified method for analysis.
Ø                  At the time interval specified in the individual monograph, withdraw a sample from a zone midway between the surface of the dissolution medium and the top of the rotating basket / paddle not less than 1cm away from the vessel wall.
Ø                  If two or more time profile is specified, then replace the aliquots withdrawn for analysis with equal volumes of fresh dissolution medium at 37°C and the volume correction shall be done in the circulation.
Ø                  Verify the temperature during the dissolution run.
Ø                  Withdrawal of aliquots shall be done within a tolerance of ± 2% of the specified time.
Ø                  Clean all the vessels and stirrers after completion of the analysis and switch OFF the instrument.

4.3              PRECAUTIONS     

Ø                  Ensure that the tank is filled with Purified / Distilled water without vessel up to the mark of the instrument, before putting on the heater switch.
Ø                  Do not over tight the paddle / basket, and also not to hold the paddle / basket when it is in operation.
Ø                  Note:   Sinkers shall be used if the dosage form unit floats. Close the vessels with the cover during Operation.

4.4              CALIBRATION 

4.4.1          PART ‘A’
Ø                  The instrument shall be calibrated for RPM and Temperature.

4.4.2          For Temperature Calibration:
Ø      Measure the temperature of the water bath and of each jar with a calibrated thermometer and compare the result against the digital display on the apparatus.
Ø      Record the observation as per Annexure – 1 (Part A) 
Ø      Acceptance Criteria: 37°C ± 0.5°C
4.4.3          For RPM Calibration.
Ø      Calibrate the apparatus at 50 and 100 RPM. Compare the RPM shown on the digital display of the apparatus with the RPM measured with a stopwatch or Taco meter.
Ø      Record the observation as per Annexure - 1
Ø      Acceptable criteria:  ± 1 RPM – for 50 RPM
                           ± 2 RPM – for 100 RPM
4.4.4          For Part B:     
·         For Wobble Calibration
Ø      Ensure that there is no significant wobbling in the shafts.
Ø      Record the observation in the format given in Annexure – 2 (Part B)
Ø      Acceptable criteria: NMT 1 mm.

 

4.4.5          PART ‘C’ 
·         Apparatus Suitability Test Disintegrating Type
Ø            Use USP dissolution calibrator disintegrating type 50 mg prednisone tablets.
Ø            This USP Dissolution Calibrator is provided for the Apparatus Suitability Test in the general chapter of USP 24 or as per the method specified in the documents received along with the respective lot of the tablet
Ø            Do not expose the tablets to excessive humidity. Store in dry, cool place.
Ø            Dissolution Media: Distilled water 500 ml.
Ø            Heat the medium with gentle stirring, to about 45° C, immediately filter under vaccum using a membrane filter, with stirring for about 5 minutes.
Ø            Weigh accurately about 10 mg of prednisone reference standard (already dried on 105°C  for 3 houre into a 100 ml volumetric flask and dissolve in 5 ml of ethanol. Make up to volume with distilled water.
Ø            Dilute 10 ml of the solution to 50 ml with distilled water.
Ø            Conduct the suitability test at conditions mentioned in the certificate of tablets using apparatus I and II.
Ø            After completion of the dissolution time withdraw filter and aliquot of the solution.
Ø            Discard the first 2 ml of solution and measure the concentration of prednisone at 242 nm against the absorbance of prednisone USP reference standard solution.
Ø            The apparatus is suitable if each of the individual calculated values for each apparatus at all indicated speed are within the specified ranges.
Ø            Record the observation as per Annexure – 3 (Part C)

·               Apparatus Suitability Test Non-disintegration Type
Ø            Apparatus suitability test for non-disintegrating type Salicylic Acid 30 mg tablets.
Ø            This USP Dissolution Calibrator is provided for the Apparatus Suitability Test in the general chapter of USP 24 or as per the method specified in the documents received along with the respective lot of the tablet.
Ø            These tablets are pure salicylic acid with no binders or fillers, because of the physical properties of such tablets, some sticking may occur during storage. Gentle tapping of the bottle may be used to separate the tablets.
Ø            Do not expose the tablets to excessive humidity. Store in a dry, cool place.
Ø            Dissolution Medium – 0.05 M phosphate buffer pH 7.4 ± 0.05, 900 ml.
Ø            Weigh accurately about 27.22 g of monobasic potassium phosphate and dilute to 1000 ml with water.  (Solution A)
Ø            Weigh accurately about 8 g sodium hydroxide and dilute to 1000 ml with water 0.2M Solution (Solution B).
Ø            Place 500 ml of solution A and 391 ml of solution B and dilute to 2000 ml with water and adjust the pH to 7.4 ± 0.05 with either of the solution A/B.
Ø            Dry a portion of salicylic acid working standard over silica gel for 3 hours before use.
Ø            Weigh accurately about 33 mg of salicylic acid working standard into a 100 ml volumetric flask, add 1 ml methanol and dissolve the powder, Dilute to volume with phosphate buffer. Dilute 5 ml to 50 ml with buffer.
Ø            Place one Salicylic acid Non-disintegrating type tablet in each of the 6 containers and operate the apparatus at each of the speeds indicated in the certificates. Withdraw and filter an aliquot of the solution
Ø            Discard the first 2 ml of solution. Dilute 5ml of the filtrate to 50 ml with dissolution medium (phosphate buffer) and measure the concentration of Salicylic acid at 296 nm against the absorbance of Salicylic acid reference standard solution.
Ø            The apparatus is suitable if each of the individual calculated values for each apparatus at all indicated speed is within the specified ranges.
Ø            Record the observation as per Annexure – 3 (Part C)

4.4.6          Frequency of Calibration         
Ø      For part A (Temperature and RPM)          -   Every 03 months
Ø      For part B (Wobble Test)                          -   Every 06 months
Ø      For part C (Apparatus Suitability)              -   Every 06 months

4.0.            REASON FOR REVISION:

Harmonization of format

6.0              TRAINING:

Trainer                         --          Head – Quality Assurance
            Trainees           --          Quality Control Chemists and Assistants 
Period               --          One day
7.0              DISTRIBUTION:

Certified Copy No.   1   :  Head of Department – Quality Control (Chemical)
Reference Copy No. 2   :  Display copy Near  Dissolution Test Apparatus (Inst. ID. No. QC/009)
Reference Copy No. 3   :  Display copy Near  Dissolution Test Apparatus (Inst. ID. No. QC/010)
Reference Copy No. 4   :  File copy in Dissolution Apparatus Calibration Data
Original Copy                :  Head – QUALITY ASSURANCE.


8.0              ANNEXURES:

            Annexure – 1    :  Format For Calibration Record Of Dissolution Test Apparatus
                                       (Temperature & RPM)
Annexure – 2    :  Format For Calibration Record Of Dissolution Test Apparatus
                           (Wobble Calibration)
Annexure – 3    :  Format For Calibration Record Of Dissolution Test Apparatus
                            (Calibration with Prednisone Tablet and Salicylic Acid Tablet)

ANNEXURE – 1

FORMAT FOR CALIBRATION RECORD OF DISSOLUTION TEST APPARATUS

REF. SOP NO.:  K/QC/020
Revision No.:  00
Page No.: 1 of 1
Effective from:
 
INSTRUMENT CALIBRATION RECORD
Name of instrument   :   Dissolution Test Apparatus
Instrument Sr. No.      :
Make & Model                      :   
Calibration Date        : 
Calibration due on      :
Part – A
  1. Temperature:
Temperature Set
(37.9°C)

Temperature Of Medium In Each Jar

Limit
1
2
3
4
5
6
37 ± 0.5 °C
By Probe






By standard thermometer






  1. Rotation Per Minute: 

RPM Set

RPM Measured

Limit
1
2
3
4
5
6
50






50 ± 1
100






100 ± 2

Remarks: Satisfactory / Not satisfactory.




Calibrated by :                                                                        Checked by:
Date :                                                                                      Date :



K/QC/020/F-1/00
           
Prepared By
Checked By
Approved By
Authorised by





ANNEXURE – 2

FORMAT FOR CALIBRATION RECORD OF DISSOLUTION TEST APPARATUS

REF. SOP NO.:  K/QC/020
Revision No.:  00
Page No.: 1 of 1
Effective from: 
Name of instrument   :   Dissolution Test Apparatus 
Instrument S. No.       :
Make & Model         :   
Calibration Date        : 
Calibration due on     :
(Part B)
Wobble Calibration       

Observed Wobble (mm)
Limit
Calibrated By
Checked By
1
2
3
4
5
6
Apparatus I






NMT 1 mm


Apparatus II







Remarks: Satisfactory / Not Satisfactory





Calibrated by :                                                                        Checked by:
Date :                                                                                      Date :                         












K/QC/020/F-2/0
Prepared By
Checked By
Approved By
Authorised by

ANNEXURE – 3

FORMAT FOR CALIBRATION RECORD OF DISSOLUTION TEST APPARATUS

REF. SOP NO.:  K/QC/020
Revision No.:  00
Page No.: 1 of 2
Effective from: 

Name of instrument   :   Dissolution Test Apparatus 
Instrument S. No.       :
Make & Model         :   
Calibration Date        : 
Calibration due on     :
Part C

I)             Calibration With Prednisone Tablet 10 mg [LOT No. _________] (Disintegration type)

Standard Preparation: __________ mg of Prednisone Standard (about 10 mg). Added __________ ml of ethanol to dissolve. Make the volume to 100 ml with water. Dilute 10 ml to 50 ml with water.

Test Dilution:  1 tablet in 500 ml of Dissolution medium (Water)
Absorbance at 242 nm :  Standard Absorbance :  _________________

App-I Abs.       :  1)  __________ 2) _________ 3) _________ 4) ________ 5) ________ 6)   ___________
App-II Abs.      :  1)  __________ 2) _________ 3) _________ 4) ________ 5) ________ 6)   ___________

Calculations:   Test abs.    X    Std. Wt.     X     10     X     500     X    100   
                           -------------------------------------------------------------------------   =      Release in %
                                    Std abs.  X    100     X     50       X     10

Apparatus
Time in Min.
RPM
Tab 1
Tab 2
Tab 3
Tab 4
Tab 5
Tab 6
Limit
Basket
30
50







Basket
30
100






Paddle
30
50







Paddle
30
100









Calibrated by :                                                                                    Checked by:
Date:                                                                                                   Date:
K/QC/020/F-3/00
Prepared By
Checked By
Approved By
Authorised by





ANNEXURE – 3

FORMAT FOR CALIBRATION RECORD OF DISSOLUTION TEST APPARATUS

REF. SOP NO.:  K/QC/020
Revision No.:  00
Page No.: 2 of 2
Effective from: 


II)          Calibration With Salicylic Acid Tablet 300 mg. [LOT No. _________] (Non-Disintegration type)

Standard preparation: __________ mg of Salicylic Acid Standard (about 33 mg). Added __________ ml of Methanol to dissolve. Make the volume to 100 ml with Buffer. Dilute 5 ml to 50 ml with Buffer.

Test Dilution: 1 tablet in 900 ml of Dissolution medium (Buffer). Dilute 5 ml to 50 ml with buffer.

Absorbance at 296: Standard Absorbance:  _________________

App-I Abs.       :  1)  __________ 2) _________ 3) _________ 4) ________ 5) ________ 6)   ___________
App-II Abs.      :  1)  __________ 2) _________ 3) _________ 4) ________ 5) ________ 6)   ___________


Calculations:        Test abs.    X    Std. Wt.     X     5     X     900     X   50    X     100   
                           ---------------------------------------------------------------------------------  =        release in %
                                           Std abs.  X    100     X     50       X     5      X    300

Apparatus
Time in Min.
RPM
Tab   1
Tab 2
Tab 3
Tab 4
Tab 5
Tab 6
Limit
Basket
30
50







Basket
30
100






Paddle
30
50







Paddle
30
100







Remarks: Satisfactory / Not satisfactory.




Calibrated by:                                                                                     Checked by:
Date:                                                                                       Date:
                              
K/QC/020/F-4/00
Prepared By
Checked By
Approved By
Authorised by

1 comment:

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