by | DEPARTMENT | : | QUALITY CONTROL |
| LOCATION | : | |
| NAME OF THE INSTRUMENT/EQUIPMENT | : | DISSOLUTION APPARATUS |
| MAKE | : | |
| MODEL/ TYPE | : | |
| INSTRUMENT/EQUIPMENT ID | : |
TABLE OF CONTENTS
| Sr. No. | Content | Page no. |
| Pre-Approval | ||
| Objective | ||
| Definitions | ||
| Scope | ||
| Qualification Team and Responsibility | ||
| Guidance table to assess the ‘Level of Qualification’ for the equipment | ||
| Acceptance of Installation qualification (IQ) | ||
| Acceptance of Operation qualification (OQ) | ||
| Acceptance of Performance qualification (PQ) | ||
| Performance Qualification (PQ) | ||
| Deviation | ||
| Abbreviation(S) | ||
| Summary and Conclusion | ||
| Attachment(S) | ||
| Hand Over Certification | ||
| Post Approval |
- Pre Approval:
Prepared By:
| Functional Area | Name | Designation | Signature/ Date |
| Quality Control |
Reviewed By:
| Functional Area | Name | Designation | Signature/Date |
| Quality Control | |||
| Quality Assurance |
Approved By:
| Functional Area | Name | Designation | Signature/Date |
| Quality-GM |
- Objective:
The purpose of Installation, Operation qualification and Performance qualification is to provide the documented evidence that the DISSOLUTION APPARATUS (Instrument ID- NA) is performing as per the parameters defined in qualification and that gives result which meet predetermined acceptance criteria.
- Definitions
- Installation qualification (IQ) is a documented verification process that the instrument or piece of equipment has been properly delivered, installed and configured according to standard set by the manufacture or by an approved installation checklist.
- Operation qualification (OQ) is establishing confidence that process equipment and sub-system are capable of consistently operating within stated limits and tolerances.
- Performance qualification (PQ) is establishing the confidence through appropriate testing that used to verify that a system perform as expected under simulated real word conditions. Under performance qualification a specified performance meets all release requirements for functionality and safety and those procedures are effective and reproducible.
- Scope:
This document covers all aspects of Installation, Operation and Performance qualification of instrument/equipment to be used.
- Qualification Team and
Responsibility:
- Quality Control:
- Prepares and reviews the document ensuring that the content is sufficient, clearly defined and technically accurate.
- Execution, Review and
verification of Installation, Operation and Performance Qualification activity
as per document.
- Quality Assurance:
- Reviews the Installation, Operation qualification and Performance qualification document.
- Ensures the proper
functioning of the instrument at designated place.
- Head– QC:
- Reviews the Installation, Operation qualification and Performance qualification document.
- Ensures the proper
functioning of the equipment at designated place.
- Quality-GM
- Review and approval of the Performance qualification document, the completed qualification data and the compiled report.
- Guide in the resolution of performance variances.
- Guidance table to assess the ‘Level of Qualification’ for the equipment is as given below.
| Category | URS | IQ | OQ | PQ | Remarks |
| Direct Impact | √ | √ | √ | √ | NA |
| Indirect Impact | √ | √ | √ | NA | PQ Shall be decided after assessment of the team based on justification |
| No Impact | NA | NA | NA | NA | PQ Shall be decided after assessment of the team based on justification |
Based on the impact of instrument/equipment qualification, the qualification of document to be performed. If No/NA; justification /reason should be provided.
| Activity Name | To be Executed (Yes/No/NA) | Justification /Reason |
| URS | ||
| IQ | ||
| OQ | ||
| PQ | ||
| Handover Certifications |
- Acceptance of Installation qualification (IQ) is performed by the Certified Service Engineer. and same to be verified and review by the Quality control person. The IQ documents provided by the service engineer and based on its acceptance criteria the installation qualification is approved by the Quality assurance person.
Performed by:
| Engineer Name | Qualification done on | Document no. | Sign/Date | Remarks |
Verified by:
| Quality Control | Qualification Verified date | Sign/Date | Remarks |
Approved by:
| Quality Assurance | Qualification Approved date | Sign/Date | Remarks |
Certification:
____________________________________________________________________________________________________________________________________________________________________________________
- Acceptance of Operation qualification (OQ: After the certification of Installation qualification, the qualification is proceeded further for the qualification and same is performed by the Certified Service Engineer . The verification of Operation qualification is verified by Quality control person. The OQ documents provided by the service engineer and based on its acceptance criteria the Operation qualification is approved by the Quality assurance person.
Performed by:
| Engineer Name | Qualification done on | Document no. | Sign/Date | Remarks |
Verified by:
| Quality Control | Qualification Verified date | Sign/Date | Remarks |
Approved by:
| Quality Assurance | Qualification Approved date | Sign/Date | Remarks |
Certification:
____________________________________________________________________________________________________________________________________________________________________________________
- Acceptance of Performance qualification (PQ) : After the certification of Operation qualification, the qualification is proceeded further for the Performance and same is performed by the Certified Service Engineer. The verification of Performance qualification is verified by Quality control person. The PQ document provided by the service engineer and based on its acceptance criteria the performance qualification is approved by the Quality assurance person.
Performed by:
| Engineer Name | Qualification done on | Document no. | Sign/Date | Remarks |
Verified by:
| Quality Control | Qualification Verified date | Sign/Date | Remarks |
Approved by:
| Quality Assurance | Qualification Approved date | Sign/Date | Remarks |
Certification:
____________________________________________________________________________________________________________________________________________________________________________________
- Performance Qualification is establishing confidence through appropriate testing that
the finished product or process produced by a specified process meets all
release requirements for functionality and safety and those procedures are
effective and reproducible.
- Calibration.
- Calibration for Auto Sampler (Sampler Calibration)
- Calibration.
Calibration of rinsing/sampling/replenishment volume:
Weigh 24 dry test tubes for rinsing and sampling volume and 12 replenishment bottles. Place 12 dry test tubes in auto sampler. 1 to 12 test tubes for rinsing volume and 13 to 24 test tubes for sampling volume. After completing the cycle of rinsing and sampling, place 12 replenishment bottles in respective position.
Then collect the volume.
Calculation:
Weight of water collected (g)
Volume collected (ml) = ————————————————-
Density of water at temperature 37.0°C
For Rinsing Volume
| Sr. No. | Weight of empty test tube (gm) | Weight of test tube + water (gm) | Volume collected ( ml ) = Weight of water collected (gm) /0.99602 | Acceptance criteria 2.0 ± 0.1ml | ||
| 1 | 1.9 ml to 2.1 ml | |||||
| 2 | ||||||
| 3 | ||||||
| 4 | ||||||
| 5 | ||||||
| 6 | ||||||
| 7 | ||||||
| 8 | ||||||
| 9 | ||||||
| 10 | ||||||
| 11 | ||||||
| 12 | ||||||
For Sampling Volume
| Sr. No. | Weight of empty test tube (gm) | Weight of test tube + water (gm) | Volume collected ( ml ) = Weight of water collected (gm) /0.99602 | Acceptance criteria 8.0 ± 0.1ml |
| 1 | 7.9 ml to 8.1 ml | |||
| 2 | ||||
| 3 | ||||
| 4 | ||||
| 5 | ||||
| 6 | ||||
| 7 | ||||
| 8 | ||||
| 9 | ||||
| 10 | ||||
| 11 | ||||
| 12 |
For Replenishment Volume
| Sr. No. | Weight of empty test tube (gm) | Weight of test tube + water (gm) | Volume collected ( ml ) = Weight of water collected (gm) /0.99602 | Acceptance criteria 8.0 ± 0.1ml |
| 1 | 7.9 ml to 8.1 ml | |||
| 2 | ||||
| 3 | ||||
| 4 | ||||
| 5 | ||||
| 6 | ||||
| 7 | ||||
| 8 | ||||
| 9 | ||||
| 10 | ||||
| 11 | ||||
| 12 |
Acceptance criteria: For rinsing volume: 2.0 ± 0.1 ml
For sampling volume: 8.0 ± 0.1 ml
For replenishment volume: 10.0 ± 0.1 ml
Density of water at temperature 37.0° C: 0.99602
For Temperature:
Fill the water as a medium in each jar and set the temperature of the Instruments 37°C and wait for half an hour.
When the Flash will glow on the LHS against ready place calibrated thermometer and RTD sensor in jar for five minutes and note down the temperature reading by calibrated thermometer and RTD sensor in the calibration record in Annexure-I and repeat this procedure for others 7 jars.
The acceptance criteria are 37° C ± 0.5°C.
| Thermometer ID | : | Calibration due on | : | |||||||
| Calibrated on | : | |||||||||
| Vessel ID | Set Temperature in °C (A) | Temperature measured by calibrated thermometer in °C (B) | Difference between A and B in °C (C) | Temperature measured by calibrated RTD Sensor in °C (D) | Difference between A and D in °C (E) | Difference between C and E in °C | Acceptance criteria in °C (37.0°C ±0.5°C) | |||
| J1 | ±0.5 | |||||||||
| J2 | ||||||||||
| J3 | ||||||||||
| J4 | ||||||||||
| J5 | ||||||||||
| J6 | ||||||||||
| J7 | ||||||||||
| J8 | ||||||||||
| J9 | ||||||||||
| J10 | ||||||||||
| J11 | ||||||||||
| J12 | ||||||||||
| J13 | ||||||||||
| J14 | ||||||||||
For RPM:
Lower the basket/Paddle by pressing “LIFT button”. Set 25 RPM on the instruments and press start RPM and rotation will start.
Measure the rotation by calibrated tachometer.
Again set the RPM at 50, 100 and 150 and measure the same by tachometer and note down the reading.
RPM Calibration: 25 RPM
| Tachometer ID No. | : | Calibration due on | : | ||
| Calibrated on | : |
| Vessel ID | Set RPM (A) | RPM measured by tachometer (B) | Difference between A and B | Acceptance criteria 25 ± 4% | ||
| J1 | ± 1 | |||||
| J2 | ||||||
| J3 | ||||||
| J4 | ||||||
| J5 | ||||||
| J6 | ||||||
| J7 | ||||||
| J8 | ||||||
| J9 | ||||||
| J10 | ||||||
| J11 | ||||||
| J12 | ||||||
| J13 | ||||||
| J14 | ||||||
RPM Calibration: 50 RPM
| Vessel ID | Set RPM (A) | RPM measured by tachometer (B) | Difference between A and B | Acceptance criteria 50 ± 4% |
| J1 | ± 2 | |||
| J2 | ||||
| J3 | ||||
| J4 | ||||
| J5 | ||||
| J6 | ||||
| J7 | ||||
| J8 | ||||
| J9 | ||||
| J10 | ||||
| J11 | ||||
| J12 | ||||
| J13 | ||||
| J14 |
RPM Calibration: 100 RPM
| Vessel ID | Set RPM (A) | RPM measured by tachometer (B) | Difference between A and B | Acceptance criteria 100 ± 4% |
| J1 | ± 4 | |||
| J2 | ||||
| J3 | ||||
| J4 | ||||
| J5 | ||||
| J6 | ||||
| J7 | ||||
| J8 | ||||
| J9 | ||||
| J10 | ||||
| J11 | ||||
| J12 | ||||
| J13 | ||||
| J14 |
RPM Calibration: 150 RPM
| Vessel ID | Set RPM (A) | RPM measured by tachometer (B) | Difference between A and B | Acceptance criteria 150 ± 4% |
| J1 | ± 6 | |||
| J2 | ||||
| J3 | ||||
| J4 | ||||
| J5 | ||||
| J6 | ||||
| J7 | ||||
| J8 | ||||
| J9 | ||||
| J10 | ||||
| J11 | ||||
| J12 | ||||
| J13 | ||||
| J14 |
The acceptance criteria: ±1 RPM (For 25 RPM), ± 2 RPM (For 50 RPM), ± 4 RPM (For 100 RPM) & ± 6 RPM (For 150 RPM).
- For Wobble (Paddle & Basket):
Set the dial gauge in the basket or paddle individually and start the rotation of the instrument at 100 RPM.
Measure the reading individually all paddles & basket and note down the reading.
| Wobble Meter ID No. | : | Calibration due on | : | ||
| Calibrated on | : |
| Sr. No. | Apparatus I- Basket shaft ID | Wobble (mm) | Apparatus II – Paddle shaft ID | Wobble (mm) |
| 1 | ||||
| 2 | ||||
| 3 | ||||
| 4 | ||||
| 5 | ||||
| 6 | ||||
| 7 | ||||
| 8 | ||||
| 9 | ||||
| 10 | ||||
| 11 | ||||
| 12 | ||||
| 13 | ||||
| 14 |
The acceptance criteria for basket are not more than 1 mm and for the paddle it is not more than 0.5mm.
- Jar Centering:
Apparatus I-Basket
Measure the distance from the shaft to the inner vessel wall at four locations equally spaced around the vessel.
( x = Xmax – Xmin).
| Vernier Caliper ID No. | : | Calibration due on | : | ||
| Calibrated on | : |
| Sr. No. | Basket shaft ID | X1 (mm) | X2 (mm) | X3 (mm) | X4 (mm) | Jar Centering DX=Xmax – Xmin |
| 1 | ||||||
| 2 | ||||||
| 3 | ||||||
| 4 | ||||||
| 5 | ||||||
| 6 | ||||||
| 7 | ||||||
| 8 | ||||||
| 9 | ||||||
| 10 | ||||||
| 11 | ||||||
| 12 |
Acceptance criteria:
| Sr. No. | (Apparatus I) | Acceptance criteria |
| 1 | Apparatus I -Basket | Less than 2.0mm |
Apparatus II-Paddle
| Sr. No. | Paddle shaft ID | X1 (mm) | X2 (mm) | X3 (mm) | X4 (mm) | Jar Centering DX=Xmax – Xmin |
| 1 | ||||||
| 2 | ||||||
| 3 | ||||||
| 4 | ||||||
| 5 | ||||||
| 6 | ||||||
| 7 | ||||||
| 8 | ||||||
| 9 | ||||||
| 10 | ||||||
| 11 | ||||||
| 12 |
Acceptance criteria:
| Sr. No. | (Apparatus II) | Acceptance criteria |
| 1 | Apparatus II -Paddle | Less than 2.0mm |
- Paddle Measurement: Apparatus II
Mark the identity on each paddle and check the physical parameter mentioned as below: Shaft diameter: 9.4-10.1 mm, Blade upper chord: 74.5 ± 0.5 mm, Blade lower chord: 42.0 ± 1.0 mm, Paddle height: 19.0 ± 0.5 mm, Paddle thickness: 4.0 ± 1.0 mm.
| Paddle Shaft ID (mm) | Shaft Diameter (9.4-10.1) | Blade Upper Chord (74.5 ± 0.5) | Blade Lower Chord (42.0 ± 1.0) | Paddle Height (19.0 ± 0.5) | Paddle Thickness (4.0 ± 1.0) |
- Basket Measurement: Apparatus I
Mark the identity on each basket and check the physical parameter mentioned as below: Shaft diameter: 9.4-10.1 mm, Total height of basket: 37.0 ± 3.0 mm, Height of open screen: 27.0 ± 1.0 mm, Internal diameter of screen: 20.2 ± 1.0 mm, External diameter of screen: 22.2 ± 1.0 mm, External diameter of ring: 25.0 ± 3.0 mm, Vent hole diameter: 2.0 ± 0.5 mm, Height of coupling disk: 5.1 ± 0.5 mm, Wire openings: 0.40 ± 0.04 mm.
| Paddle Shaft ID (mm) | Shaft Diameter (9.4-10.1) | Total Height of Basket (37.0 ± 3.0) | Height of Open Screen (27.0 ± 1.0) | Internal Diameter of Screen (20.2 ± 1.0) | External Diameter of Screen (22.2 ± 1.0) |
| Paddle Shaft ID (mm) | External Diameter of Ring (25.0 ± 3.0) | Vent Hole Diameter (2.0 ± 0.5 mm) | Height of Coupling Disk (5.1 ± 0.5 mm) | Wire Openings (0.40 ± 0.04) |
- Distance between Bottom edge of Basket (D1) & Paddle (D2)
Measure the distance between inside bottom of the vessels & basket/ paddle with depth gauge and note down the observation in calibration format.
| Depth gauge ID No. | : | Calibration due on | : | ||
| Calibrated on | : |
| Sr. No. | Vessel ID | Measured paddle height (mm) | Measured basket height (mm) | Acceptance criteria: 25 ± 2mm |
| 1 | 23 mm to 27 mm | |||
| 2 | ||||
| 3 | ||||
| 4 | ||||
| 5 | ||||
| 6 | ||||
| 7 | ||||
| 8 | ||||
| 9 | ||||
| 10 | ||||
| 11 | ||||
| 12 | ||||
| 13 | ||||
| 14 |
The acceptance criteria are 25 ± 2mm for basket & paddle.
- For Timer:
Set the timer of the instrument at 10 minutes, 30 minutes, 60 minutes and 120 minutes and RPM at 50. Start the RPM and stop watch simultaneously. Record the time of stop watch at each time point
| Stop watch ID No | : | Calibration due on | : | ||
| Calibrated on | : |
| Sr. No. | Set time (A) | Observed time (B) | Difference between A and B | Acceptance criteria |
| 1 | 10 Minutes | ±30seconds | ||
| 2 | 30 Minutes | |||
| 3 | 60 Minutes | |||
| 4 | 120 Minutes |
The acceptance criteria are ±30 seconds.
- Performance verification Test (Two-stage test as per certificate of Prednisone Tablets USP)
Dissolution medium preparation:
Heat a suitable amount of water at about 45°C, sonicate for 10 minutes to degas. Filter under vacuum through a 0.45µm porosity filter. Transfer the media into the dissolution vessel. Set the temperature at 37°±0.5°C. The temperature of the dissolution medium should not fall below 37°C prior to the initiation of the test.
The adopted test method is single stage test as per USP. Following are the dissolution conditions:
Apparatus : Type-1 (Basket) & Type-2 (Paddle)
Medium : 500 ml Water
Medium Temp : 37°±0.5°C
Time : 30 Minutes
RPM : 50RPM
Wavelength : 242nm
Standard preparation:
Take 10 mg of Prednisone USP reference standard in a 100 ml volumetric flask, add 5 ml of ethanol and sonicate to dissolve and make up to the volume with water. Further dilute 10.0 ml of this solution to 100.0 ml with water.
Sample preparation:
After getting the required temperature, place Prednisone one tablet each in eight/twelve dissolution vessel. And after the completion of the test, pipette out the sample from each vessel with cannula midway between the surface of dissolution medium and the top of the rotating basket/paddle not less than 10 mm from wall of the vessel. Take 10 ml of the test solution. Filter the solution with 0.45µm porosity filter. Dilute 5.0 ml of this solution to 10.0 ml with water.
Take the absorbance of standard and sample solution at 242 nm
Calculation:
Sample Absorbance Standard weight 10 500 10 Potency
= ————————— x ———————- x —— x ——– x —– x ——– x 100
Standard Absorbance 100 100 10 5 100
For geometric mean and coefficient of variation, use the excel sheet provided by the USP.
If results not meet the acceptance criteria of 1st stage of two stages then go to 2nd stage of two stage and results should meet the acceptance criteria as given in certificate of Prednisone tablets USP.
Standard weight :.…….( 10mg) → 5 ml Ethanol+ 95ml water (100ml) → 10ml → 100ml with water.
Test Dilution: 1 Tablet → 500 ml water → 5ml →10ml water
Standard Absorbance at 242nm :
:
Set – 1 Set – 2 (Additional set of Tablets)
| Type-1 (Basket) | Type-1 (Basket) | |||||
| Sr. No. | Absorbance | % Release | Sr. No | Absorbance | % Release | |
| 1. | 1. | |||||
| 2. | 2. | |||||
| 3. | 3. | |||||
| 4. | 4. | |||||
| 5. | 5. | |||||
| 6. | 6. | |||||
| 7. | 7. | |||||
| 8. | 8. | |||||
| 9. | 9. | |||||
| 10. | 10. | |||||
| 11. | 11. | |||||
| 12. | 12. | |||||
| 13. | 13. | |||||
| 14. | 14. |
Set – 1 Set – 2 (Additional set of Tablets)
| Type-2 (Paddle) | Type-2 (Paddle) | |||||
| Sr. No. | Absorbance | % Release | Sr. No | Absorbance | % Release | |
| 1. | 1. | |||||
| 2. | 2. | |||||
| 3. | 3. | |||||
| 4. | 4. | |||||
| 5. | 5. | |||||
| 6. | 6. | |||||
| 7. | 7. | |||||
| 8. | 8. | |||||
| 9. | 9. | |||||
| 10. | 10. | |||||
| 11. | 11. | |||||
| 12. | 12. | |||||
| 13. | 13. | |||||
| 14. | 14. |
* Calculation: Spl. Abs. x Std wt. x 10 x 500 x 10 x Potency x 100
Std. Abs. 100 100 10 5 100
*Calculation sheet attached / not attached.
For Geometric mean and coefficient of variation use the excel sheet available on USP official website.
Geometric mean=……………………………………
.
Coefficient of Variation=…………………………….
Remark: The observed values complies / does not comply the acceptance criteria and the equipment can be / cannot be used for routine analysis.
Performed by
Name:
Sign/Date
Performance Qualification done by/date ____________ Checked by/date _______________
- Frequency of Calibration
All Physical Parameter Calibration: Three Months ± 07 days.
Performance Verification Test: Six Months ± 15 Days.
- DEVIATION:
Report any deficiencies from the acceptance criteria or from protocol instructions. Record the brief description in the table below. Include all deficiency report forms. Indicate the completeness checked by sign and date after resolving of the deficiency.
Deviation observed (if any)
______________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________
Action taken (if any)
______________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________
Justification for acceptance:
______________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________
- ABBREVIATION(S):
SOP : Standard Operating Procedure
QA : Quality Assurance
HOD : Head of department
QC : Quality Control
IQ : Installation Qualification
OQ : Operational Qualification
PQ : Performance Qualification
NA : Not applicable
mg : Milligram
gm : gram
% : Percentage
- Summary and conclusion:
__________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________
Prepared By: ___________________________________________ __________________
Name / Department Sign. / Date
- Attachment(S):
| Sr. No. | Annexure No. | Document Title |
Remarks: ____________________________________________________________________________________________________________________________________________________________________________________
Verified By: ________________ (Sign./Date)
- Handover Certification:
This DISSOLUTION APPARATUS bearing Instrument/Equipment ID………………… qualification is completed on dated ………………… and has been installed in wet laboratory ………………… by the certified service engineer . The qualification has been verified against the criticality of the instrument and it meets/does not meet the acceptance criteria.
Hence the DISSOLUTION APPARATUS is certified /not certified for routine operation .
- Post Approval:
Executed By:
| Functional Area | Name | Designation | Signature/ Date |
| Quality Control |
Reviewed By:
| Functional Area | Name | Designation | Signature/Date |
| Quality Assurance | |||
| Head Quality Control |
Approved By:
| Functional Area | Name | Designation | Signature/Date |
| Quality-GM |
