1.0 Objective

To describe the Operational Qualification of Double Cone Blender and to define the specification of the system in order to:

• Ensure that the equipment meets the Operational/Design limits.

• Demonstrate that the equipment / system will perform reproducibly and consistently within its full range of operation according to manufacturer’s specification

• Ensure that the equipment will be operationally qualified in accordance with current Good Manufacturing Practices

• Assure that the equipment / system performance is adequate to support the process for which the system is intended.

• Demonstrate that the suitability of the SOP is established for the equipment / system

2.0 Scope

The scope of this document applies to the operational qualification of Double Cone Blender installed in granulation area.

5.0 Operational Qualification Test Matrix

The following test(s) / verifications must be completed successfully for a satisfactory

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1.0 PURPOSE

The purpose of performance qualification is to confirm through the provision of objective evidence, that the performance requirements for the Coating Machine with equipment ID.: XXXXXXXXXXX meet its intended use. 

2.0 SCOPE

The preparation of PQ applies to the Coating Machine installed in Coating area of YYYYYYY with equipment ID.: XXXXXXXXX.

3.0 PROCEDURE FOR PERFORMANCE QUALIFICATION

3.1 Flow output verification of the peristaltic Pump

3.1.1 Scope: The observed RPM value of the peristaltic pump shall be monitored for compliance with respective to its set values in the MMI.

3.1.2 Methodology/Sampling Plan

• Operate the Coating machine as per SOP.
• Collect solution in the solution holding tank and connect the inlet of the peristaltic pump on to the outlet valve of the tank.
• Set the RPM of the peristaltic pump at a particulate value in the MMI.
• Attach sample covers onto nozzle and collect the quantity of solution out in one minute.
• Seal the covers and weigh individually to get the flow rate (ml/min) from each nozzle at a particular set RPM of the peristaltic pump.
• Record the observation in table I given in this protocol.

3.1.3 Acceptance criteria:

• The observation RPM value of the peristaltic pump shall comply with its set value.
• The flow output shall be consistent from all nozzles. (For information purpose only)

3.2 Spray Pattern Checks.

3.2.1 Scope: The minimum atomization air pressure required to produce a cone-shaped spray pattern with suitable width at a particular RPM value of the peristaltic pump shall be recorded for information purpose only.                                                  

3.3 Methodology/Sampling plan:

• Operate the Coating Machine as per SOP
• Set the RPM of the Peristaltic pump at a particulate value and operate to start flow of solution from the nozzles.
• Apply atomization air pressure gradually till a cone shaped spray pattern with a suitable width at a particular RPM setting of the peristaltic pump.
• Record the atomization air pressure to achieve a cone shaped spray pattern with a suitable width at a particular RPM setting of the peristaltic pump.
• Record the observation in the table 2given in this protocol.

3.3.1 Acceptance criteria:

• A cone shaped spray shall be observed (For information purpose only)

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1.0 Overview

The Performance Re-Qualification of Fluid Bed Dryer is carrying out in order to provide the high degree of assurance that the equipment performed as intended and remain in the state of control.

2.0 Purpose

The purpose is to provide an outline for the Performance Re-qualification of equipment for performance attributes to verify that:

• Documented the verification of all aspects of the equipment that can affect product quality.

• To make an impact assessment of the critical components of the equipment’s on the material.

• To establish, check and document the performance of equipment in the established/predetermined operating ranges.

• The protocol shall define the test procedures, documentation, references and acceptance criteria to establish that the performance of the equipment shall meet the predetermined acceptance criteria.

• The equipment shall be used for the homogeneous drying of the wet mass with the help of hot air drying and fluidization process.

3.0 Background

The Fluid Bed Dryer supplied by Falcon Machineries, Equipment I.D. XXXX installed in Granulation at XYZ (Company Name) This protocol defines the methods and documentation that shall be used to evaluate the performance attributes of Fluid Bed Dryer. The Reason for this requalification is Periodic/Schedule Performance Requalification.

4.0 Performance Re-Qualification Procedure

The following procedure shall be used for performance of Fluid Bed Dryer:

• Training shall be imparted to the concerned personal on Performance Re-Qualification protocol.
• Operate the machine as per respective standard operating procedure and set the required parameter in control panel as per product BMR.
• Record the observation in the protocol.
• The equipment shall be challenged with charging of Wet granulated material manufactured as per BMR. equipment.
• Drying of Material is done as per parameters mentioned in the Batch Manufacturing record.
• Sample for LOD shall be done from the 06 different location mentioned in protocol
• Record the Results of LOD in respective section given in the protocol.
• Sample quantity shall be collected approximately 2 g in at each location.
• All data shall be recorded in respective BMR and results shall be recorded in report observation table.
• Suitable conclusion shall be drawn after completion of Performance Re-Qualification.
• Any deviation observed during qualification shall be recorded in the observed deviation, corrective action and justification report section.
• Observed deviation shall be reported to the department head and quality head.
• If the observed deviation does not have any major impact on the qualification the final conclusion shall be provided.
• If the observed deviation has major impact on the qualification, deviation shall be reported to the manufacturer for the corrective action and qualification activity shall be done.

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1.0 Overview

The Performance Re-Qualification of Rapid Mixer Granulator is carrying out in order to provide the high degree of assurance that the equipment performed as per functional specification and remain in the state of control.

2.0 Purpose

The purpose is to provide an outline for the Performance Re-Qualification of equipment for performance attributes to verify that:

• Documented the verification of all aspects of the equipment that can affect product quality.

• To make an impact assessment of the critical components of the equipment’s on the material.

• To establish, check and document the performance of equipment in the established/predetermined operating ranges.

• The protocol shall define the test procedures, documentation, references and acceptance criteria to establish that the performance of the equipment shall meet the predetermined acceptance criteria.

• The equipment shall be used for the homogeneous mixing of the dry material and wet kneading by mixing and crushing the material with the help of high shear force accomplished by agitator.

3.0 Background

The Rapid Mixer Granulator supplied by Falcon Machineries, Equipment I.D. XXXXX installed in Granulation at XYZ (Company Name).  This protocol defines the methods and documentation that shall be used to evaluate the performance attributes of Rapid Mixer Granulator in accordance with the URS specifications and intended use. The Reason for this requalification is Periodic/Schedule Performance Requalification

4.0 Performance Re-Qualification Procedure:

The following procedure shall be used for Requalification of Rapid Mixer Granulator:

• Training shall be imparted to the concerned personal on Performance Re-Qualification protocol.
• Operate the machine as per respective standard operating procedure and set the required parameter in control panel as per product BMR.
• Record the observation in the protocol.
• The equipment shall be challenged by using wet granulation product manufacturing process
• All the data shall be recorded in Batch manufacturing record.
• All the raw materials after sifting through the specified sieve are collected in the double lined polybags. The Rapid mixer granulator is charged with the material the quantity of which is mentioned in the bill of material.
• Dry mixing shall be carried out at slow RPM of impeller.
• After dry mixed, materials shall be used for granulation by using a freshly prepared binder. The binder shall be added to the dry mix blend at a uniform rate and the end point is decided by observing the coherent mass.
• The capacity of the rapid mixer granulator is 250 L as per the manufacturer’s specification.
• The performance of the equipment is challenged by charging with wet mass.
• All data shall be recorded in respective BMR and results shall be recorded in report observation table.
• The granulated mass shall be collected in the trolley and is taken for drying in the fluidized bed dryer.
• Suitable conclusion shall be drawn after completion of Performance Re-Qualification.
• Any deviation observed during qualification shall be recorded in the observed deviation, corrective action and justification report section.
• Observed deviation shall be reported to the department head and quality head.
• If the observed deviation does not have any major impact on the qualification the final conclusion shall be provided.
• If the observed deviation has major impact on the qualification, deviation shall be reported to the manufacturer for the corrective action and qualification activity shall be done

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1.0 Overview

The Performance Re-Qualification of Octagonal Blender is carrying out in order to provide the high degree of assurance that the equipment performed as intended and remain in the state of control.

2.0 Purpose

The purpose is to provide an outline for the Performance Re-Qualification of equipment for performance attributes to verify that:

• The system meets the user requirement Specification.

• Document the verification that equipment performs consistently and in the state of control.

• Assure that Octagonal Blender is adequate to support the process for which the system is intended.

3.0 Background

The Octagonal Blender supplied by Falcon Machineries; Equipment I.D. XXXX installed in Blending area at XYZ (Company Name). This protocol defines the methods and documentation that shall be used to evaluate the performance attributes of Octagonal Blender in accordance with the user requirement specifications and intended use. The Reason for this requalification is Periodic/Schedule Performance Requalification.

4.0 Performance Re-Qualification Procedure

The following procedure shall be used for Requalification of Octagonal Blender:

• Training shall be imparted to the concerned personal on Performance Re-Qualification protocol.

• Verification of performance of machine done by Blending of material.

• Operate the machine as per respective standard operating procedure and set the required parameter in control panel as per product BMR.

• Record the observation in the protocol.

• Sample for Blend uniformity shall be done from the 10 different locations mentioned in protocol

• One composite sample shall be taken from Blender

• Record the Results of Analysis in respective section given in the protocol.

• The Performance of Octagonal blender shall be evaluated for minimum and maximum load.

• Suitable conclusion shall be drawn after completion of Performance Re-Qualification.

• Any deviation observed during qualification shall be recorded in the observed deviation, corrective action and justification report section.

• Observed deviation shall be reported to the department head and quality head.

• If the observed deviation does not have any major impact on the qualification the final conclusion shall be provided.

• If the observed deviation has major impact on the qualification, deviation shall be reported to the manufacturer for the corrective action and qualification activity shall be done.

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1.0 Overview

The Performance Re-Qualification of Compression Machine is carrying out in order to provide the high degree of assurance that the equipment performed as intended and remain in the state of control..

2.0 Purpose

The purpose is to provide an outline for the Performance Re-Qualification of equipment to verify that:

• The system meets the user requirement Specification.
• Document the verification that equipment performs consistently and in the state of control.
• Assure that Compression Machine 27 Station is adequate to support the process for which the system is intended.

3.0 Background

The Compression Machine supplied by Fluidpack, Equipment I.D. XXXXX installed in Compression area at XYZ (Company Name). This protocol defines the methods and documentation that shall be used to evaluate the performance attributes of Compression Machine in accordance with the user requirement specifications and intended use. The Reason for this requalification is Periodic/Schedule Performance Requalification.

4.0 Performance Re-Qualification Procedure

The following procedure shall be used for Requalification of Compression Machine:

• Training shall be imparted to the concerned personal on Performance Re-Qualification protocol.
• Verification of performance of machine done by monitoring the physical parameters of the product at the tablet compression stage.
• The performance verification of compression machine check at different speed, different thickness pressure and different level of powder in hopper.
• Operate the machine as per respective standard operating procedure and set the required parameter in control panel as per product BMR.
• Record the observation in the protocol.
• Any deviation observed during qualification shall be recorded in the observed deviation, corrective action and justification report section.
•  Observed deviation shall be reported to the department head and quality head.
• If the observed deviation does not have any major impact on the qualification the final conclusion shall be provided.
• If the observed deviation has major impact on the qualification, deviation shall be reported to the manufacturer for the corrective action and qualification activity shall be done.

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1.0 OBJECTIVE:

The objective of Performance Requalification is to establish the documented evidence that the Sterilizing and Depyrogenating Tunnel performing consistently, reproducibly and remains in the state of controls.

2.0 SCOPE

This protocol is applicable for Performance Requalification of Sterilizing and Depyrogenating Tunnel (ID No. ____________) and its associated activities for the subject equipment.

3.0 PROCEDURE

3.1 Air Velocity Monitoring Test:

3.1.1 Objective:

To ensure that the air system is balanced and capable of delivering sufficient air volumes to maintain a minimum cross-sectional velocity under the HEPA filters when directly monitored from HMI during heat distribution and heat penetration runs as per acceptance limit.

3.1.2 Preconditions

Equipment running in normal mode

3.1.3 Necessary Materials

Calibrated Annemometer

3.1.4 Procedure:

• Switch on the depyrogenating tunnel
• Switch ON the blowers of depyrogenating Tunnel, keep the heater off
• Measure the Air Velocity at the four corners and centre of the filter at the distance of working surface from filter grill. Calculate and record the average velocity.
• Record the air velocity details of Tunnel HEPA Filter as per Attachment-III

3.1.5 Acceptance criteria

1. For drying zone average velocity should be 120± 20% FPM (0.6 M/Sec ± 20%) in the entire HEPA filter area
2. For hot sterilizing zone average velocity should be 160± 20% FPM (0.8 M/Sec ± 20%) in the entire HEPA filter area
3. For cool zone average velocity should be 100± 20% FPM (0.5 M/Sec ± 20%) in the entire HEPA filter area

3.2 HEPA Filter integrity Test

3.2.1 Objective

To ensure HEPA filter are free of defects and pin hole leaks

3.2.2 Preconditions

Equipment running in normal mode

3.2.3 Necessary Materials

• PAO smoke generator
• Aerosol photometer, duly calibrated with national/international traceability

3.2.4 Procedure

• Switch on the depyrogenation tunnel
• Switch on the blower oft he depyrogenation tunnel and keep the heater off
• Introduce the PAO cloud/aerosol as a challenge agent into the upstream side oft he HEPA filter system within the range of 20-80 µg/Litre concentration and detect the concentration with the help of aerosol photometer.
• Set the photometer upstream concentration to 100%
• Once the 100% setting is established at the upstream side turn the instrument knob to down stream. Remove the HEPA filter grill and keep the scaning probe one inch below the HEPA filter face, and start scanning the HEPA filter face area and fitment of HEPA filter with frame.
• If any leak is observed then assure that the leakage is coming through the fitment part or HEPA filter itself.
• If fitment leakage is there, tightening the HEPA filter fitment with pressure plate can arrest it and if the HEPA filter leakage is still there, the joint can be sealed by silicon sealant, but it should not exceed 1% oft he total surface area.
• Same procedure follow fort he integrity of exhaust filter.
• The results shall be recorded in the data sheet  Attachment-IV

​3.2.5 Acceptance criteria

• The upstream concentration shall be within the range of 20-80 µg/l
• Scanning should be performed over the entire downstream face of each HEPA filter and seal between the filter frame and the grid structure, including its joints, with an appropriate photometer square probe should not exceed 5 cm/s. With a rectangular probe, the maximum area scan should not exceed 15cm2/Sec.
• Aerosol at the downsteram oft he HEPA filter surfaceand joints should be detected less than 0.01% of upsteram concentration.

3.3 Air Borne Particle Monitoring Test:

3.3.1 Objective

To ensure that the Air Flow through HEPA filter is capable to maintain the predefined cleanliness class.

3.3.2 Necessary Materials

Calibrated Air Borne Particle Counter and Paper rolls.

3.3.3 Preconditions

Equipment is in normal operation mode

3.3.4 Procedure

• The cleanliness class verification is done using a calibrated Air borne Particle counter at rest phase
• Using calibrated air borne article counter find the particle count
• The test shall be carried at three locations for each zones.
• Carry out the studies with Empty Tunnel.
• The temperature of Sterilizing Chamber of the Tunnel should not be more than
• 5 ⁰ C above the ambient temperature during the test
• Switch "ON" the Blowers of the tunnel. Keep the Heaters "OFF". Let the blowers run for 30 minutes for zones stabilization.
• Place the receptor probe at working height from the surface and periphery of each HEPA Filter
• Operate the Particle Counter as per SOP, Programme the particle counter to take one cubic meter sample each from the locations as defined in following Figure No. 1

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1.0 OBJECTIVE

This protocol is designed to establish sufficient data, to assure that the Autoclave is suitable for Terminal Sterilization of the defined load patterns when operated in accordance with the established standard operating procedure.

2.0 SCOPE

This Performance Requalification Protocol is applicable for the Autoclave (Terminal Sterilizer) installed in Production (Ampoule-Injection).

3.0 Vacuum Leak test  

3.1 Objective

To establish that the leak rate is within the acceptable limit after attachment of external sensors which will assure that during temperature distribution or penetration study there will be no air entrapment due to leaks at probe locations and hence no air pocket inside the Autoclave. This will give assurance of proper heat distribution or penetration during the terminal sterilization cycle.

3.2 Procedure

• The Autoclave is equipped with automatic systems that performs the steps below automatically & calculates the leak rate (pressure rise in mbar/ min) automatically.
• This test will be performed in the following conditions/ situations during the RQ study:
• 01 run; with external sensors for validation study inserted into the chamber.
• 01 run; after removing the external sensors inserted for the validation study (at the end of the PQ study).
• Set the vacuum leak test cycle on the controller of the equipment & operate the equipment as per respective SOP for “Operation, Cleaning and Maintenance of Autoclave”.

Attached Annexures:

1.0 Signature log-Annexure-I

2.0 Vacuum Leak Test-Annexure-II

3.0 Empty Chamber Heat Distribution Studies.-Annexure-III

4.0 Loaded Chamber Heat Penetration Studies.-Annexure-IV

5.0 Deviation Details-Annexure-V

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1.0 OBJECTIVE

The objective of this protocol is to be described the procedure and plan for validation of washing of different sizes of glass Ampoules using Ampoules washing machine and to demonstrate that Ampoules washing machine shall perform washing of different sizes of glass Ampoules which meets the desired meet acceptance criteria in a consistent manner when operated as per the standard operating procedure.

2.0 SCOPE:

The scope of this protocol is limited to the validation of Ampoules washing process for different sizes of glass Ampoules.

3.0 PERFORMANCE QUALIFICATION TEST PLAN

3.1 Performance qualification test shall include following test:

3.1.1Performance Test Matrix

ENCLOSED DOCUMENTS

Following documents are enclosed as part of Performance requalification protocol and shall be preapproved as a part of the main protocol.

1.0 OBJECTIVE

This protocol is designed to establish sufficient data, to assure that the Autoclave is suitable for Sterilization of the defined load patterns when operated in accordance with the established standard operating procedure.

2.0 SCOPE

This Performance Requalification Protocol is applicable for the Autoclave installed in Production (Ampoule-Injection).

8.0 Vacuum Leak test  

8.1 Objective

To establish that the leak rate is within the acceptable limit after attachment of external sensors which will assure that during temperature distribution or penetration study there will be no air entrapment due to leaks at probe locations and hence no air pocket inside the Autoclave. This will give assurance of proper heat distribution or penetration during the sterilization cycle.

8.2 Procedure

• The Autoclave is equipped with automatic systems that performs the steps below automatically & calculates the leak rate (pressure rise in mbar/ min) automatically.
• This test will be performed in the following conditions/ situations during the RQ study:
• 01 run; with external sensors for validation study inserted into the chamber.
• 01 run; after removing the external sensors inserted for the validation study (at the end of the PQ study).
• Set the vacuum leak test cycle on the controller of the equipment & operate the equipment as per respective SOP for “Operation, Cleaning and Maintenance of Autoclave”.
• Observe and record the time (T1) and the pressure (P1).
• Wait for 300 sec ± 10 sec and not more than 600 sec ± 10 sec, to allow evaporation of condensed water in the chamber and vacuum hold time started, then observe and record the pressure (P2) in the chamber and the time (T2) .
• After a further 600 sec ± 10 sec, observe and record the pressure (P3) and the time (T3).
• Allow the cycle to proceed normally to completion.
• Calculate rate of Vacuum leak rate as per equation below –

                  Where- LR = Vacuum leak rate in mbar / minute

                               P₃   = Final pressure in the chamber in mbar

                  P₂ = Pressure in the chamber after stabilization in mbar

• Record the observations in Attached annexure-II.

8.3 Acceptance criteria

• Leak test Rate should not be more than 1.3 mbar per minute.

9.0 Bowie-Dick test

9.1 Objective

To ensure that the vacuum pulses applied before the sterilization hold period are sufficient to remove the entrapped air or non-condensable gases so as to facilitate rapid and even steam penetration into all parts of the load and maintaining these conditions for the specified temperature holding time.

9.2 Materials Required

• Bowie Dick Test Kit
• Calibrated Data logger
• Calibrated temperature sensor.

9.3 Test Description

• Perform this test using readymade Bowie–Dick test pack, at a set sterilization temperature of 121°C.
• Select the Bowie-Dick test cycle from the HMI. Set the sterilization hold time as per manufacturer recommendation for Bowie Dick pack.
• Operate the equipment as per respective SOP.
• When the cycle is complete, remove the indicator paper from the test pack and observe for colour change.
• Mark the details on the paper viz. the load number, cycle number, data etc. and attach the same to the protocol.
• In case of improper colour change rectify the equipment; repeat the tests as per procedure mentioned above. Do not use the equipment till the fault has been rectified.
• Record the observations & data as per Annexure-III.
• Attach the cycle printout along with this data sheet.

9.4 Acceptance criteria

Visual indication of the cycle completion should be there at the end of the cycle.

There should be a uniform color change over the entire pattern of the indicator sheet. No change, non-uniform change and/ or air entrapment (bubble) spot on the pattern indicates inadequate air removal from the sterilization chamber

ATTACHMENTS:

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