

Pharmaceutical Updates was started to share knowledge among the pharma professionals & it will become helpful to the pharma Professionals. The author of pharmaceutical updates is Chandrasekhar panda who is having more than 13 years of Experience in Pharmaceutical Quality Assurance department and he has worked in Pharma Companies like Cipla, USV & Aurobindo Pharma Limited.
Month: January 2021
1.1 Objective is to record the findings of qualification study executed as per pre-approved protocol and to show that the digital weighing balance stands qualified for routine use.
2.1 The scope of this report is limited to Digital Weighing Balance having Id No. XYZ
3.0 RESPONSIBILITIES:
Maintenance Officer/Executive: To prepare qualification protocol, report and co-ordinate the entire qualification activity.
Quality Assurance Officer/Executive: To witness the qualification study and ascertain that the study is conducted as per the protocol.
Production Officer/Executive: To execute qualification study in co-ordination with other departments.
Head Maintenance: To review the qualification documents.
Head Quality Assurance: To approve the qualification documents.
4.0 BALANCE DESCRIPTION:
Sr. No. | ID. No. | Capacity | Least count | Location | Make | Model No. | Serial No. |
1 | XYZ | Max. : 50.00 Kg Min. : 0.50 Kg | 0.01 Kg | Packing Hall | Mettler Toledo | NA | Example: ABCD |
5.0 ACCEPTANCE CRITERIA:
Qualification of the equipment should meet the acceptance criteria outlined in the following steps.
5.1 Installation Verification Report
Sr. No. | Check points | Acceptance criteria | Observations | Checked by sign/date |
1 | Check the levelling of the equipment on level indicator. | Air bubble shall be at centre position of level indicator. | ||
2 | Placing location | 1. Bench top or floor shall be steady and even surface. 2. Location shall be free from heat, vibration and moisture. |
5.2 Multimeter Calibration Verification Report
Sr. No. | Measuring Device | Acceptance Criteria | ID. No. | Calibration done On & due on | Observation | Checked by Sign/ Date |
Multimeter | It shall be calibrated for its performance. |
5.3 Calibration Status of Standard Weights
Sr. No. | Standard Weights | Acceptance criteria | Observation | Checked by sign/date |
1 | Check the calibration of standard weights. | Standard weights should be calibrated for its performance. |
5.4 Operational Verification Report
Sr. No. | Check points | Acceptance criteria | Observations | Checked by sign/date |
1 | Press ‘Φ’ button. | Balance should turn ON. | ||
2 | Press ‘T’ button. | Balance should tare (zero – setting). | ||
3 | Press ‘Φ’ button. | Balance should turn OFF. |
5.5 Utility Verification Report
Sr. No. | Utility | Acceptance criteria | Observation | Checked by sign/date |
1 | Electricity | Single phase, 230 + 10% V AC and 50 + 5% Hz |
5.6 Eccentricity Test Report
5.6.1 Procedure
Eccentricity test is carried out by placing 1/3 rd weight of maximum capacity i.e. 20.00 Kg on weighing platform at 5 different locations (four corners & center) and Values displayed by Balance against standard weight are recorded in a following table.
Location ID | Standard Weights | Observation/Weight Displayed | Checked by sign/date |
1 | 20.00 Kg | ||
2 | 20.00 Kg | ||
3 | 20.00 Kg | ||
4 | 20.00 Kg | ||
5 | 20.00 Kg |
5.7 Linearity Test Report
5.7.1 Procedure
Linearity test is carried out by placing 4 different standard weights i.e. 0.50 Kg, 15.00 Kg, 30.00 Kg and 50.00 Kg one by one on weighing platform in ascending order and by removing the placed standard weights in descending order. Values displayed by Balance against standard weights area recorded in a following table
Sr. No. | Standard Weights | Observation/Weight Displayed | Checked by sign/date |
A | Ascending order | ||
1 | 0.50 Kg | ||
2 | 15.00 Kg | ||
3 | 30.00 Kg | ||
4 | 50.00 Kg | ||
B | Descending order | ||
1 | 50.00 Kg | ||
2 | 30.00 Kg | ||
3 | 15.00 Kg | ||
4 | 0.50 Kg |
14.98 Kg to 15.02 Kg for 15.00 Kg
29.97 Kg to 30.03 Kg for 30.00 Kg
49.95 Kg to 50.05 Kg for 50.00 Kg
5.8 Repeatability Test Report
5.8.1 Procedure:
Repeatability test is carried out by placing minimum i.e. 0.50 Kg, optimum i.e. 25.00 Kg and maximum i.e. 50.00 Kg weight of capacity of balance 5 times on weighing platform and values displayed by Balance against standard weight are recorded in a following table.
Sr. No. | Standard Weights | Observation/Weight Displayed | Checked by sign/date |
1 | 0.50 Kg | ||
2 | 0.50 Kg | ||
3 | 0.50 Kg | ||
4 | 0.50 Kg | ||
5 | 0.50 Kg | ||
6 | 25.00 Kg | ||
7 | 25.00 Kg | ||
8 | 25.00 Kg | ||
9 | 25.00 Kg | ||
10 | 25.00 Kg | ||
11 | 50.00 Kg | ||
12 | 50.00 Kg | ||
13 | 50.00 Kg | ||
14 | 50.00 Kg | ||
15 | 50.00 Kg |
24.97 Kg to 25.02 Kg for 25.00 Kg
49.95 Kg to 50.05 Kg for 50.00 Kg
6.0 DEVIATION REPORT:
Sr. No. | Deviation (s) | Justification for acceptance criteria | Impact on installation, operation and performance |
7.0 CHANGE CONTROL:
8.0 LIST OF ANNEXURE:
9.0 SUMMARY AND CONCLUSION OF QUALIFICATION
10.0 CERTIFICATION OF QUALIFICATION:
Qualification is satisfactory. Yes/No
Hence Balance can be used for routine use. Yes/No
Head- Q.A.
Objective of this report is to provide documented evidence through the verification of installation, operation & performance of Tablet Friability Tester to show that the instrument installed, operated and consistently performed according to predetermine specifications.
The scope of this Report is limited to Id No. XYZ
3.0 QUALIFICATION TEAM AND RESPONSIBILITIES:
DEPARTMENT | NAME & SIGNATURE | RESPONSIBILITY |
Maintenance | To prepare qualification report. To co-ordinate the entire qualification activity. | |
Quality Assurance | To execute qualification study in co-ordination with other departments. | |
Production | To execute qualification study in co-ordination with other departments. | |
Maintenance | To review the qualification documents. | |
Head – Quality Assurance | To approve qualification protocol & report. |
4.0 INSTRUMENT DESCRIPTION:
For instrument description, should match as per re qualification protocol
5.0 ACCEPTANCE CRITERIA:
Qualification of the instrument shall be in accordance with the parameters given in Annexures – A, B, C, D, E, F, G, H, I & J of this report.
6.0 OBSERVATIONS:
Qualification shall be executed using following forms:
Annexure- A
INSTALATION VERIFICATION CHECK LIST
Sr. No | Checks to be performed | Acceptance criteria | Observation | Checked by/Date |
1 | Check for the receipt of the consignment. | It shall be received in good condition. | ||
2 | Check for any scratches on the machine body and drums. | It shall not have any scratches on machine body and drums. | ||
3 | Check for electrical connection | It shall not observed a loose or damage connection. | ||
4 | Check for levelling of the platform. | Air bubble of level indicator should be at centre. | ||
5 | Check both drums are properly locked with knob on the shaft. | Both drums should be properly locked with knob on the shaft. |
Annexure- B
CALIBRATION OF MEASURING DEVICES
Sr. No. | Measuring devices | Acceptance criteria | Observation | Checked by/Date |
1 | Vernier Calliper | It should be calibrated within calibration period. | ||
2 | Thermometer | It should be calibrated within calibration period. | ||
3 | Stopwatch | It should be calibrated within calibration period. | ||
4 | Multimeter | It should be calibrated within calibration period. |
Annexure- C
SITE INSPECTION CHECKLIST
Sr.No. | Parameter | Acceptance criteria | Observation | Checked by/ Date |
1 | Room Temperature | 15 to 30°C | ||
2 | Room Humidity | 40 to 70 % RH | ||
3 | Room environmental checks | – Away from direct sunlight. – Free from vibration. – No corrosive gases. – Free from excess dust and moisture. | ||
4 | Table space | Width :15” Length : 18” Height : 20” |
Sr.No. | Parameter | Acceptance criteria | Observation | Checked by/ Date |
5 | Point for electrical connection | Single phase of 230 V AC 50 Hz | ||
6 | Base/table level | Levelled sturdy, with no vibration. | ||
7 | Earthing | Shall be provided. |
Annexure- D
UTILITY VERIFICATION CHECKLIST
Sr.No | Parameter | Acceptance criteria | Observation | Checked by/Date |
1 | Phase Voltage: | Single Phase, 220/230 VAC, 50/60 Hz. |
Annexure- E
TECHNICAL SPECIFICATION CHECKLIST
Sr. No. | Test | Acceptance criteria | Observation | Checked by/ Date |
1 | Speed | 25 Revolutions per minute (RPM) | ||
2 | Speed Accuracy | ± 1 RPM | ||
3 | Time range | 01 Sec. to 09 Hrs.59 Min. 59 Sec. | ||
4 | Count Range | 01 to 99999 revolutions. | ||
5 | Motor | DC Stepper Motor of 3.5 KgCm Torque, 6 Volts | ||
6 | Type of the Drum | Electrolab AD Drum and Abrasion Drum. | ||
7 | Power Supply | Single Phase, 220/230 V AC, 50/60 Hz | ||
8 | Fuse Rating | T 160 mAmp – (For I/P Supply as 220/230 V AC, 50/60 Hz) | ||
9 | Dimension | 350mm (L) X 310mm | ||
10 | Weight | 12 Kg. (approx.) | ||
11 | No. of Drums | 02 Nos. | ||
12 | No. of Discharge Trays | 02 Nos. |
Annexure- F
DRUMS SPECIFICATION CHECK LIST
Sr. No. | Name | Acceptance criteria (As per USP General Chapter – 1216) | Observation | Checked by / Date | ||
1 | Drums | – One side removable. | ||||
— | — | — | Drum 1 and Drum 2 | — | ||
– | Material | Transparent synthetic polymer with polished internal surfaces. | ||||
– | Inside Radius of Curved Projection | 80.5 ± 5.0 mm. | ||||
– | Diameter of Central Hole | 10.0 ± 0.1 mm. | ||||
– | Diameter of Central Ring | 25.0 ± 0.5 mm. | ||||
– | Inside Diameter of Drum | 287.0 ± 4.0 mm. | ||||
– | Outside Diameter of Drum | 302.5 ± 4.0 mm. | ||||
– | Depth of Drum | 38.0 ± 2.0 mm. | ||||
– | Tablet Dropping Height | 156.0 ± 2.0 mm. | ||||
– | – | – | – |
Annexure- G
OPERATIONL VERIFICATION CHECKLIST
Sr. No. | Operation | Acceptance criteria | Observations | Checked by/ Date |
1 | Switch ‘ON’ the power switch. | – The drum shall initialize itself to the loading position. – The display shall now show ‘Start” | ||
2 | a) Press ‘TIME’ key to select the “TIME MODE”. | – The MODE indicator LED shall indicate the “TIME MODE”. -The display shall show the previous time values. | ||
b) Enter the desired value by using numerical keys. Press ‘ENTER’ key to register the value. | The display shall show ‘00’. | |||
c) Press ‘RUN/HALT’ key. | – The drum shall start rotating in forward direction. – The display shall show elapsed time. – When the test is over the drum shall rotate in reverse direction for discharging the tablets into the tray. – Indication of test over shall show by an audible beep. – The display shall show “END”. | |||
d) Press ‘RESET’ key. | The instrument shall initialize and will stop at the loading position. | |||
3 | a) Press ‘COUNT’ key to select the “COUNT MODE”. | – The MODE indicator LED shall indicate the “COUNT MODE”. – The display shall show the previous count values. | ||
b) Enter the desired value by using numerical keys. Press ‘ENTER’ key to register the value. | The display shall show ‘00’. | |||
c) Press ‘RUN/HALT’ key. | – The drum shall start rotating in forward direction. – The display shall show elapsed count. – When the test is over the drum shall rotate in reverse direction for discharging the tablets into the tray. – Indication of test over shall show by an audible beep. – The test over shall show “END”. | |||
d) Press ‘RESET’ key. | The instrument shall initialize and the will stop at the loading position. |
Sr.No | Test procedure | Acceptance criteria | Observation | Checked by/Date |
1 | Start the instrument. | Instrument shall run. | ||
2 | Turn main power to the instrument OFF. | The instrument shall get OFF. | ||
3 | Turn Power ON. | Instrument should not start spontaneously. | ||
4 | Start the instrument. | Instrument should resumes from the stop condition with all the parametrs found as before POWER – OFF. |
a) For regular tumbling, set the instrument at normal position, as there is no any irregular tumbling of tablets.
b) For irregular tumbling, set the instrument with 10° tilt with the bench top to prevent any irregular tumbling of tablets.
1.1 Acceptance criteria: Performance of instrument shall be found satisfactory.
1.2 For Normal Position:
Product Name:
Batch No.:
Sr. No. | Time Set in Minute | Initial weight | Final weight | Friability | Checked by/Date |
1 | |||||
2 | |||||
3 |
1.3 For 10° Tilt Position:
Product Name:
Batch No.:
Sr. No. | Time Set in Minute | Initial weight | Final weight | Friability | Checked by/Date |
1 | |||||
2 | |||||
3 |
7.0 DEVIATION REPORT:
Sr. No. | Deviation (s) | Justification for acceptance criteria | Impact on installation, operation and performance |
8.0 CHANGE CONTROL:
9.0 LIST OF ANNEXURE:
10.0 SUMMARY AND CONCLUSION OF QUALIFICATION:
11.0 CERTIFICATION OF QUALIFICATION:
Qualification is satisfactory Yes/No
Hence instrument can be used for routine use. Yes/No
Objective of this report is to check and provide documented evidence of its performance as per the predetermined acceptance criteria.
Refer working and principle of RMG https://pharmaceuticalupdates.com/2020/04/27/working-and-principle-of-rapid-mixer-granulator-rmg/
2. SCOPE:
The scope of this report is limited to equipment ID No. XYZ.
3. QUALIFICATION TEAM AND RESPONSIBILITIES:
DEPARTMENT | NAME AND SIGNATURE | RESPONSIBILITY |
Quality Assurance | To prepare performance qualification protocol and report. To co-ordinate the entire qualification activity. | |
Production | To execute qualification study in co-ordination with other departments. | |
Quality Assurance | To execute qualification study in co-ordination with other departments. | |
Maintenance | To review the qualification documents. | |
Head – Quality Assurance | To approve qualification protocol & report. |
4. EQUIPMENT DESCRIPTION:
Equipment description shall be match as per design qualification protocol.
5. ACCEPTANCE CRITERIA:
Performance Qualification of the equipment shall be in accordance with the parameters given in FORM – A of this report.
6. PROCEDURE:
Perform the qualification as per following form,
Performance of Equipment
PERFORMANCE OF EQUIPMENT
Performance of the equipment is verified by simulating the normal operation for dry mixing, granulation and milling of the ingredients. While doing the exercise consideration is given to the operational range of the equipment that is at minimum level (20% of capacity), optimum level (50% of the capacity) and maximum level (80% of the capacity). At the end of the granulation process wet mass is checked for its physical appearance.
1.0 Minimum Level: (20 % of capacity)
Product Name :
Batch No. :
Theoretical Batch Size :
Practical Batch Size :
1.1 Dry Mixing:
Uniform mixing of raw materials i.e. active and inactive materials is checked by collecting samples from 10 different locations for blend uniformity test. The result of blend uniformity test, process parameters of equipment i.e. mixer speed, chopper speed and end point ampere reading are recorded in following tables.
1.1.1 Acceptance Criteria:
Mixing of active material shall be uniform.
Blend Uniformity: 90.0 % to 110.0 %
% RSD: NMT 6.0 %
1.1.2 Process Parameters Data:
sr no. | Step | Mixer Slow | Mixer Fast | Chopper Slow | Chopper Fast | End Point Ampere | Observation entered by/date |
1 | Dry mixing cycle |
1.1.3 Blend Uniformity Test Result:
Sr. No. | Locations | Assay in % | Result entered by/date |
1 | Left – Top | ||
2 | Left – Bottom | ||
3 | Right – Top | ||
4 | Right – Bottom | ||
5 | Middle – Top | ||
6 | Middle – Bottom | ||
7 | Front – Top | ||
8 | Front – Bottom | ||
9 | Back – Top | ||
10 | Back – Bottom | ||
Minimum | |||
Maximum | |||
Average | |||
% RSD |
1.2 Wet Mixing (Binder Addition):
After addition of binder solution, checked the wet mass, process parameters of equipment i.e. binder solution temperature, mixer speed, chopper speed and end point ampere reading. The observations are recorded in following tables.
1.2.1 Acceptance Criteria: Wet mass shall be coherent.
1.2.2 Process Parameters Data:
Binder solution temperature:
Sr No. | Steps | Mixer Slow | Mixer Fast | Chopper Slow | Chopper Fast | End Point Ampere | Observation entered by/date |
1 | During binder solution addition. | ||||||
2 | After completion of binder solution addition. | ||||||
3 | Additional purified water, if added. Quantity : |
1.2.3 Physical Appearance of Wet Mass:
Sr.No. | Test | Observation | Checked by/date |
1 | Physical appearance |
The wet mass after granulation is passed though the cone mill and the same is checked visually for its size and uniformity.
1.3.1 Acceptance Criteria: Wet granules size shall be uniform.
1.3.2 Physical Appearance of Wet Mass:
Sieve details:
Sr.No. | Test | Observation | Checked by/date |
1 | Visually check wet granules for its size. |
Repeat the above mentioned process for optimum level (50% of the capacity) and maximum level (80% of the capacity).
7. Deviation Report:
Any deviation reported during process with respect to acceptance criteria shall be justified and it’s it’s impact on equipment qualification shall be evaluated.
8. CHANGE CONTROL:
Change control number shall be mentioned.
9. List of Annexures:
Annexures shall be attached to the PQ Report.
10. Summary and Conclusion of Performance Qualification:
The results and final conclusion shall be mentioned that the equipment performance is found satisfactory at load condition and analytical and physical parameters performed at different capacities are found satisfactory.
11. Certification of Performance Qualification:
Performance Qualification is satisfactory Yes/No
Hence equipment can be used for routine use Yes/No.
Certification shall be taken from Quality Assurance before use.