Process Performance Qual PDF

Process Performance Qualification Protocol for Autoclave : Pharmaceutical Guidelines Page 1 of 13
Process Performance Qualification Protocol for Autoclave

Validation Protocol of Autoclave (Steam Sterilizer) Sterilization Process i.e Autoclaving
1.0 Objective:
The objective of this protocol is to verify the performance qualification attributes i.e. sterilization and to establish sufficient data to assure that the S
STERILIZER (Equipment ID No.) supplied by M/s, XYZis suitable for sterilizing planned load.
To prepare master chart of sterilization cycle for reference during normal production cycle.
To demonstrate that Autoclave is leak proof and there is no leakage from the chamber.
To ensure that system is capable to remove air pocket from Autoclave chamber.
To ensure that heat distribution throughout the chamber is uniform and the temperature is within the limit of 121 to 123C.
To ensure that the heat is sufficiently penetrating into the innermost portions of the load subjected for sterilization to achieve a temperature of 12
123C during the Sterilization hold period.
To ensure that the steam Sterilization process, when challenged withGeobacillus StereothermophilusBiological indicator spore strips having spore
population of 10 spores strip, should reduce the bacterial load by more than 6 log reduction.
6
Related:Low Temperature Sterilization Process (115C)
2.0 Scope:
This Protocol shall be applicable to theAutoclave(Equipment No.:ABCD), situated in the clean room no. A10 in the plant of ..Company
atcity.
3.0 References:
3.1 Internal References
Sr. No.
01
02
03
04
05
06
07
Reference Detail
Operation of Kaye Validator
Calibration of Measuring & Testing Devices
Operation of HTR
Operation of Valprobe loggers
Handling of Biological Indicator
Risk Management
Deviation Management
Document No.
Reference Detail
Scottish Health Technical
Document No.
SHTM 2010
3.2 Others
Sr. No.
01
Memorandum 2010, Part 3 of 6,

Validation and verification
02
03
Sterilization, June 2001

BRITISH STANDARDBS EN, Sterilization Steam
sterilizers Large sterilizers (The European Standard EN
285: 1996)
Industrial Moist Heat Sterilization
PDA Journal of
In Autoclaves
Pharmaceutical
PDA Technical Monograph No. 1,
04
EN 285
Science and
2005 Revision Supplement, Volume 59, Number X

Sterilization of health care products Moist heat Part
2: Guidance on the application of ANSI/AAMI/ISO 17665-1
Technology
ANSI/AAMI/ISO
17665-1
4.0 Responsibilities:
Department
Quality
Assurance
Responsibilities
Q.A. Officer / Executive:
http://www.pharmaguideline.com/2012/10/process-performance-qualification.html
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To prepare/review standard operating procedure/protocol as per current

GMP requirement and organizations Quality norms.
To ensure & follow correct procedure written in SOP & protocol.
Ensure the sampling instruction written in Protocol is followed to
withdrawsample at specified location in specified time interval and
witness of validation activity.
Test the collected product sample tested as per specification.
To report any abnormality to QA Manager / QAHead and take
corrective and preventive action in coordination with respective
department head.
Q.A. Manager:
Review & Approval of Protocol & Report.
Ensure all the raw data generated were in accordance with protocol &
expected results achieved.
Head - Q.A./ President-Technology:
Technical
Department
Manufacturing
Review and approval of protocol and validation report.

Executive / Manager Technical:Is responsible for review & scheduling
the planned validation activity and to provide technical support for
execution of protocol.
Manufacturing Chemist:To follow instruction written in SOP
Production Manager/ Q.A. Manager
Ensure implementation of BMR and protocol.
Ensure the sample were withdrawn & sent to the QC for testing as per
specification.
Ensure all the equipment used during Process validation was
documented in respective equipment usage log.
5.0 Frequency:
5.1 Initial Validation:
Three (3) successful runs for all planned loads.

5.1.1 Shifting of the equipment from one location to another location.
5.1.2 If replacement of major components / Instruments.
5.1.3 Change in PLC programme.
5.2 Revalidation:
One successful run once in a year for all loads at defined maximum load pattern.
6.0 Rationales for Validation Study:
6.1 Rationales for Probes quantity
6.1.1 Empty chamber Heat Distribution:

In steam sterilization process steam is not flowing, only condensate formed in the chamber is purged out and the pressure in the chamber is maint
further inlet of steam. Therefore uniform heat distribution is expected in the steam sterilizer chamber during sterilization hold period and prob
non-uniformity within the chamber is less.
In the Autoclave steam inlet is from the both sides of the chamber through baffles, for uniform distribution of steam in the chamber. Condensate dr
point is located at the bottom. Three horizontal planes of two shelves (i.e. top and bottom) are selected for temperature mapping.4 probes to be p
four corners of top shelves, 3 probes at corner &1 probe at centre of top selves. 3 probes at corner & 1 probe in drain point of lower shelves (attach
6.1.2 Loaded chamber heat penetration:
For sterilization of Rubber stoppers, Garment & Miscellaneous Load (Silicone tube) the 5 probes are placed inside the load, 1 probe in drain po
probes in the chamber as per respective loading pattern diagram attached as Exhibits to this protocol for monitoring of heat penetration in
chamber.
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Once the maximum and minimum load are validated for Autoclave at defined validated Load pattern need not to qualify periodically for minim
Therefore only maximum loads will be periodically revalidated at defined load pattern considering it as worst case scenario.
6.2 Process Parameter:
Key operating parameters as per Operational Qualification identified are as below:

Sr. No.
Parameter Details
Pure Steam Pressure
Vacuum
Compressed Air
Process Parameter
NLT 2.0 Bar (g)
NLT 0.70 Bar (g)
NLT 6.0 Bar (g)
6.3 Functional Risk Assessment
Function wise processes are listed and evaluated for assessment of risk to either product quality and data integrity. It involves mainly following step
1. Identifying GMP Risk
2. Identifying Risk Scenarios
3. Assessing the likelihood of An Adverse Event
4. Assessing the severity of impact
5. Detection of adverse impact
6. Overall priority
The above risk were prioritization of risk in High/Medium/Low categories.
6.4 Identifying GMP Risk
System function parameters are evaluated and identified whether they represent a risk when assessed against a series of GMP criteria.
Following types of risks are mainly identified during risk assessment process for qualification of system as below:
Risks towards non-availability of required documentation
Risks towards non-availability of required SOPs
Risks towards non-availability of system Access Control
Risks towards abnormal user operation performed at the time of system operation
Risks towards incorrect configuration of system
Risks towards Improper and/or inadequate training
6.5 Identifying Risk Scenarios
Having determined that a particular function may have a GMP risk associated with it, the assessment proceeds to identify the various risk scenarios
events that identify the risks associated with use of the system.
The functions identified are analyzed by considering possible hazards/adverse effects and what controls may be needed to minimize the potential h
6.6 Assessing the Likelihood of An Adverse Event
After identifying hazards / adverse events, determine the likelihood (frequency or probability) of it occurring. User considers the likelihood of the ad
event occurring per number of transactions, and assigns category as per estimation of risk.
6.7 Assessing the Severity of Impact
After determining likelihood of adverse event, severity of its impact on process is assessed. These effects take into account impact on re
compliance, impact on product quality and impact on data integrity.
The impact of risk occurring may be described as follows:
6.8 Ranking of Adverse Event Severity
Table - I
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Value
3
2
1
(S) Severity of Event (Consequence)

High(H) : Can cause serious adverse health consequences which can
threaten the life of Patient or even death
Medium(M) : Temporary or reversible adverse health consequences
but the life of the patient is not threatened
Low(L) : No effect/Impact for patients
6.9 Detection of Adverse Event
Next step is to identify if the adverse event can be recognized or detected by other means in the system. Adverse event having high prob
detection, may not pose a serious threat because it can be recognized quickly and suitable corrective action taken to mitigate its impact. If an adve
has a low probability of detection, then the risk condition needs to seriously consider a review of the design or the implementation of al
procedures to avoid the event.
6.10 Ranking of Adverse Event Detection
Table - II
Value
1
2
3
(D) Level of Detection

High (H): The risk can be easily detected through deployed control
measure/system and the detection system is automated.
Medium (M): The risk can be detected later through deployed control
measure/system and the detection is through manual method.
Low (L): The risk cannot be detected through deployed control
measure/system the detection is possible after longer period/interval.
6.11 Risk Review and Monitor Controls
After controls are implemented, they will be monitored for life cycle of the system. This will be part of performance monitoring of the system.
review after the system is fully operational /validated shall
a.Consider whether previously unrecognized risks are present
b.Determine if previously identified hazards are still present ( and to what level)
c.Ascertain if the estimated risk associated with a hazard is no longer acceptable
d.Evaluate whether all existing controls are still necessary
6.12 Risk Assessment & Control During Execution of study:
6.12.1Nature of Risk & its mitigation action to the risk identified:

Sr.
No
Description of Risk
Identified
Impact
Level of Risk
after mitigation
plan
(Low /
Moderate / High)
Risk of System Access by Unauthorized/untrained personnel
1
Unauthorized person Process may gets
Low
tries to conduct the
affected.
process.
Untrained operator
tries to
operate /maintenance
of the system.
Operation SOP does
not contain proper
information.
Process may gets

affected.
Low
Expected results
Observation
Tested
By
(Sign &
Date)
Only Qualified persons

are authorized to perform
the process and conduct
the study
Training plan, training
record and Operation
SOP should be available.
Process may gets

affected.
System operation SOP

should contain operation
3
Low
information as
recommended by QA.
Risk on account of abnormal process condition occurred at the time of system operation
Failure of Vacuum
Process gets
Low
Message appears on
leak test
affected.
PLC Leak Test Fail.
4
SOP contains
information to take action
accordingly.
Low
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Sr.
No
Description of Risk
Identified
Impact
Level of Risk
after mitigation
plan
Expected results
Observation
(Sign &
Date)
(Low /
Moderate / High)
Failure of Bowie Dick
Test
Process gets
affected.
Tested
By
Fail is having indication

of light color in center of
pattern
SOP contains
accordingly.
Failure of Biological
Process gets
Low
Indicator.
affected.
Risk on account of abnormality in connected utilities at the time of system operation
If Pure steam
Process gets
Pressure and hence
pressure Low during
affected.
temperature not achieve
running cycle.
in the system.
6
Low
Low vacuum
SOP contains
accordingly.
Result in Atypical cycle
Process gets
affected.
Low
Temperature lower
during sterilization
running the cycle.
Process gets
affected.
Low
SOP contains
accordingly.
Temperature not
achieve in the system.
10
11
Temperature higher
during sterilization
phase of cycle.
May System loss

or damage to
components
Low
Load is not placed as

per defined and
validated load pattern
Load may not

get sterile
Low
SOP contains
accordingly.
SOP contains
accordingly.
SOP contains
accordingly.
12
Authorized and trained
person is performing the
operation.
Risk occurred in Equipment
Door gaskets
Process gets
damaged
affected.
Low
13
Malfunctioning of
pneumatic valves
Process gets
affected.
Low
14
Malfunctioning of
Steam trap
15
Chamber vacuum not

maintained
Process gets
affected.
Low
SOP contains
accordingly.
SOP contains
accordingly.
Temperature not
achieve in the system
SOP contains
accordingly.
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Sr.
No
16
Description of Risk
Identified
Failure of post
calibration of
thermocouple.
Impact
Could not
accessed about
product
sterilization
Level of Risk
after mitigation
plan
(Low /
Moderate / High)
Low
Expected results
Observation
Tested
By
(Sign &
Date)
Result of BI will be
assessed for probability
of survival of
microorganisms.
Check physical
condition of
thermocouples if found
damage, white proper
justification.
Recalibration to be
done.
7.0 Equipments/ Material to be used for Validation Study:
Calibrated Valprobe loggers/Thermocouples

Kaye Valprobe/Kaye Validator
Calibration Unit
Biological Indicator
Media to incubate
Chart paper (Yokogawa)
Bowie Dick Pack
7.1 Technical Data
Mfg. By:
Installed on:
Model no.:
Size:
Working Pressure:
Volume:
Door:
Hydraulic test Pressure:
Construction:
The Autoclave consists of the following features.
TheAutoclaveChamber is made up of Stainless Steel sheet, which is welded with a U-Profile Stainless Steel Jacket. TheAutoclaveChamber is provi
two sliding doors, which are also made up of Stainless Steel reinforced with mild steel support structure. The door is operated with the help of pn
cylinder, when the door reaches the end position gaskets are pushed out automatically with help of compressed air for sealing similarly to open
gasket is retracted by vacuum. When the gasket is retracted the door slides automatically. The Door sealing is done with the help of tubular, silicon
gasket. To ensure proper sealing the gaskets are activated with compressed air and retracted with the help of vacuum.
Door interlocks are provided to prevent simultaneous opening of both the doors of critical area side (sterile area side) and controlled area side (no
area side) and process lock to prevent opening of the door during the operation.
TheAutoclavechamber is insulated with resin-bonded glass wool, which helps in reducing the heat loss to the environment and ensuring
distribution of temperature inside the chamber. This insulation is covered with stainless steel cover plate.
A Stainless steel pipe stand support is provided for the equipment thus requiring no special foundation. For ensuring leak tight partition betw
Controlled area (Non-Sterile area side) and Clean area (Sterile area side), a Stainless steel flush paneling is provided on the partitioning wall and t
cover ofAutoclave. All Joints, Crevices are filled with Silicon sealant to prevent any leakage.
TheAutoclaveis provided with the following systems and accessories for proper functioning.
Water-ring type vacuum pump with suitable electric motor.
Vacuum break filter on the clean area side. One pair of removable Stainless Steel railings inside the sterilization chamber for smooth and easy ope
the load article.
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Loading tray constructed of Stainless steel SS316.

Chamber Compound gauge on sterile and Controlled area side, Jacket pressure gauge of the Controlled area side, Gasket compound gauge for bo
doors on the Controlled area side and critical area side, Safety valve for jacket and chamber, Steam trap with strainer and NRV for chamber.
Pure steam is supplied through SS-316 piping from generation center installed at WFI generation room.
Control panel consisting of PLC, Digital Temperature input to the microprocessor from a 5 Nos of Temperature transmitters, one Pressure transmi
Pressure and vacuum switches for giving digital pressure/vacuum signals to the microprocessor, Manual backup system for operation in case of
microprocessor failure.
Stainless steel Internal Piping, Ball valves with rotary actuators for all the process lines with solenoid valves to regulate air supply to the pneumatic
actuators.
7.2 Monitoring and Controlling of the sterilization cycle:
7.2.1TwoPT-100 probes, inserted in Chamber to monitor temperature on yokogawa recorder.

7.2.2One similar PT-100 probe is left in the drain by which cycle is controlled by PLC. Temperature of drain shall be monitored on PLC and at y
recorder.
7.3 Study Design:
Name of the
Study
S. No.
1
Recipe
Vacuum leak test
No. of trials
to be taken
Leak Test
One
Bowie Dick Cycle
Bowie-Dick
One
Empty chamber Heat Distribution
HPHV RSD
One
HPHV RSD
One
HPHV RSD
One
HPHV RSD
One
Loaded chamber with Rubber

Stoppers
Loaded chamber with garment and
hand gloves
Loaded chamber with Miscellaneous
items (Silicone tube)
4
5
6
Note: -Newload may be introduce in loading pattern in between two scheduled re- qualification study after three successful validation run and rep
same shall be attached as addendum to last validation report.*
Reference cycle detail (Initial validation with Protocol No)
Sr. No.
1
2
3
Protocol No.
Protocol No.
Heat Penetration study in Rubber closure RFS

(Ready For Sterilization) bag (Applicable for 20
mm rubber stopper)
Heat Penetration study for Garment
Sterilization
Heat Penetration study for Miscellaneous Load
7.4 Sterilization Cycle Parameters:
Sr. No
Name of Parameter
Leak test
Vacuum Leak Test
Programme Name
1.
2.
Select Cycle (Recipe No)
3.
Leak Vacuum on
4.
Vacuum Hold
4
2
-0.7 kg/cm
15 min
7.5 Recipe For Bowie Dick Cycle:
Sr. No
Bowie Dick
Test
Name of Parameter
1.
2.
3.
Initial vacuum time

Pulsation
2 min
3
4.
Preheating Temperature
95C
5.
Preheating Time
1 min
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6.
7.
8.
9.
10.
11.
Sterile Temperature
Sterile Time
121.0 C
10 min
Sterile Print Time

Dry Vacuum Time
Dry Vacuum Value
1 min
0 min
Door
Temperature
-0.700 Kg/cm
Open 90 deg
7.6 Recipe For HPHV RSD cycle:
Sr. No
Name of Parameter
Value
1.
2.
Initial Vacuum Pulse
3.
Initial Vacuum Value
500 mm of Hg
4.
5.
Initial vacuum time

Preheating Temperature
6.
Preheating Time
7.
Sterile Temperature
2 min
95 C
1 min
121.0 C
8.
Sterile Time
15 min
9.
Sterile Hold Print Time
60 sec
10.
Dry Vacuum Pulse
11.
Dry Vacuum Value
600 mm of Hg
20 min
12.
Dry Vacuum Time
13.
JKT STM PRE REL
14.
Cool Vacuum Value
600 mm of Hg
15.
Cool Vacuum Time
5 min
16.
Jacket Air vent ON
5 sec
17.
Jacket Air vent OFF
12 sec
18.
Jacket Air Pressure Rel
1 min
19.
Door Open Temperature
90 deg
2 min
8.0 Procedure:
8.1 Vacuum leak test Procedure:
8.1.1Put the flexible probes inside the chamber through the validation port provided for the validation cycles prior to start of Vacuum leak test.
8.1.2Ensure that Autoclave is empty and chamber is at ambient temperature.
8.1.3Ensure compressed air is ON at required pressure of 6 bar.
8.1.4Ensure sufficient water supply is available for seal of vacuum pump
8.1.5Ensure gasket lubrication is proper
8.1.6Switch ON Main switch provided on panel board.
8.1.7Close loading side door by pressing Door 1 close Push button provided on main panel board.
8.1.8 Ensure chart recorder is ON & graph is properly loaded.
8.1.9Check the programme from control panel.
8.1.10Enter the Operator level password & enter the programme as per requirement.
8.1.11Select programme by pressing Enter Key F1 once.
8.1.12All parameter will start on displaying on screen one by one.
8.1.13Enter F1 button and select programme, the display will show YES-1 NO-2.
8.1.14Checks the online printer attached to PLC & then select 1 and press Enter.
8.1.15Cycle will start in automatic mode as per set parameter as PLC will show Leak Test Vac ON and vacuum will be created in chamber.
8.1.16After completion of hold period, vacuum release valve will open and message will display Leak Test Vac Release and continue till the
pressure comes to atmospheric pressure.
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8.1.17At the end of the cycle, if the leak rate is more than 1 mm of Hg/ min during hold period, then message will display Leak Test Fail & if it is
1 mm of Hg/min during hold period, then message will display Leak Test Pass.
8.1.18If cycle fails, initiate work request form for rectification of problem.
8.1.19After rectification of problem fresh cycle to be run. Upon completion of cycle screen will display Cycle Over.
8.1.20Continue to run for next cycle of Bowie-Dick test.
8.2 Bowie Dick test Procedure:
8.2.1Load the tray in the autoclave chamber.

8.2.2Place the Bowie-Dick test pack on the bottom shelf of the sterilizer just above the drain point (Nearly 100 mm over the drain).
8.2.3Selected the recipe Bowie-Dick test cycle from MMI/HMI display as per point no 8.1.10 to 8.1.12. Ensure that sterilization hold time is 10 mi
121C. (Manufacturers recommendation).
8.2.4Start the cycle by pressing Enter key.
8.2.5After the cycle is over, open the door from control area side & take the sterilized test pack from the Autoclave and check the indicator paper
uniform color change.
8.2.6Observation should be recorded in test data sheet no 05 (Exhibit II).
8.2.7A Fail is indicated by light color in the center of the pattern than around the edges when compared with control.
8.2.8Failure of the pattern to change completely black or dark brown at 121 C when compared with control.
8.3 Procedure For Empty Chamber Heat Distribution Study
8.3.1Connect the calibrated thermocouples with SIM to the Kaye Validator and distribute these thermocouple through out chamber as per Exhibit-I
8.3.2Operate Kaye Validator as per SOP or Val probe logger as per SOP.
8.3.3Run HPHV RSD cycle as per SOP with recipe defined in point 7.6.
8.3.4Select the cycle from the MMI/ HMI panel as per point no.8.1.10 to 8.1.12 & start HPHV RSD cycle as well as start Kaye Validator at same ti
data at every 10 sec interval in Validator.
8.3.5After completion of the cycle take the printout of report generated through Kaye Validator. Evaluate the report as per acceptance criteria.
8.3.6Attach the report generated through Kaye Validator and PLC print out & graph from chart less recorder to the report.
8.4 HEAT PENETRATION STUDIES
8.4.1 Procedure For Loaded chamber heat penetration study:

8.4.1.1Load the articles into Double door Autoclave as per their respective loading diagram attached as exhibit to this protocol.
8.4.1.2Place heat penetration probes inside the loaded articles and select the positions where heat penetration is difficult.
8.4.1.3Connect the Thermocouple with SIM to Kaye Validator as per SOP or Val probe logger as per SOP, which senses the temperature.
6
8.4.1.4Place biological indicator folded with aluminum foil strips of Geobacillus Stereothermophilus containing 10 spores along with flexible probe
8.4.1.5Select the HPHV RSD cycle as per point no. 8.1.10 to 8.1.12.
8.4.1.6Start the cycle by pressing Enter key from the MMI / HMI panel as well as start Kaye Validator at same time. Scan data at every 10 sec interva
Validator.
8.4.1.7After completion of the cycle take the printout of report generated through Kaye Validator. Evaluate the report as per acceptance criteria
8.4.1.8Carry out total three replicate runs with loaded chamber for newly introduced load (first time study).
8.4.1.9Take out all exposed biological indicator strips & send the biological indicator to microbiological lab for testing as per SOP of handling of bi
indicators and recording the results in observation sheet.
8.4.2 Heat Penetration Study: Maximum Load of 20mm Rubber Stopper in RFS Bag (Ready For Sterilization)
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Process Performance Qualification Protocol for Autoclave : Pharmaceutical Guideli... Page 10 of 13
8.4.2.1Load the 20 mm rubber stopper [(1) 5000 Nos. x 5 bags = 25,000 nos. OR (2) 2500 nos. x 10 bags = 25,000 nos.] packed in Rexam pack read
sterilization in the chamber of autoclave in two trays as per defined loading diagram attached with this protocol.
8.4.3 Heat Penetration Study: Minimum Load of 20mm Rubber Stopper in RFS Bag
8.4.3.1Load the 20 mm rubber stopper (2500 nos. x 1 bags = 2,500 nos.) packed in Rexam pack ready for sterilization in the chamber of autoclave i
trays as per defined loading diagram attached with this protocol.
8.4.4 Heat Penetration Study: Garment Sterilization with Maximum Load
8.4.4.1Load the 32 numbers of garment packed in baby bag & 32 goggle for sterilization in the chamber of autoclave in two trays as per defined
diagram attached (Exhibit VIII) with this protocol.
8.5 Heat Penetration Study: Garment Sterilization with Minimum Load
8.5.1Load the 5 numbers of garment packed in baby bag & 5 goggle for sterilization in the chamber of autoclave in two trays as per defined
diagram attached (Exhibit IX) with this protocol.
8.6 Heat Penetration Study: Miscellaneous Load (Silicone Tube)
8.6.1Ensure cleaning of Silicone tube before packing in Rexam bag.

8.6.2Keep the silicone pipe (Approx 2 meter long) in Rexam bag by folding in circular way, keeping both end open.
8.6.3Insert the biological Indicator folded with aluminum foil along with Thermocouple in both end of silicone tube. Insert the probe as long a
inside the tube. Care should be taken when insertion that after sterilization the biological indicator should be removed easily.
8.6.4Load the 4 number of silicone tube packed in Rexam pack ready for sterilization in the chamber of autoclave in two trays as per defined
diagram attached with this protocol.
8.7 Load Configuration:
01
Load
No
NA
02
NA
Sr. No
Name of the
Load
Leak Test
Bowie Dick
Test
Load Pattern
Load Type
NA
NA
No of
Articles
NA
Bowie Dick
NA
1 No
Maximum
25,000 Nos
Minimum
2,500 Nos
20 mm Rubber
Stopper
03
04
Rubber
Stopper
Rubber
Stopper
05
10
Garment Load
06
11
Garment Load
07
12
Miscellaneous
Load
(5000 nos x 05
bags)
or (2500 nos x 10
bags)
20 mm Rubber
Stopper
(2500 nos x 1
bag)
Garment Bags
Goggle
Garment Bags
Goggle
Maximum
Silicon tube
NA
Minimum
32
32
5
5
4
Note:
1.During validation study, if there is any change required in the type and/ number of articles to be loaded, loading diagram will be changed. A
validation result the diagrams will be established for routine cycles and accordingly SOP will be established. In this case protocol will not be re
validation method will remain same.
8.8 Attachments to Report:
8.8.1
Attachment 01: Common for all tests
Calibration Report of Thermocouples

Calibration Verification Report of Thermocouples
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8.8.2
Attachment 02: For Leak Test Cycle
Yokogawa Graph
PLC print
8.8.3
Attachment 03: For Bowie-Dick Test
Test Indicator Paper

Yokogawa Graph
PLC print
8.8.4
Attachment 04: For Heat Distribution Study
Standard Format: VAL/STR/1.4

Yokogawa Graph
PLC print
Thermocouples set up Report
Thermocouples Qualification Report
8.8.5
Attachment 05: For Heat Penetration Study for 20mm Rubber Stopper Maximum Load
Standard Format: for logging data

Yokogawa Graph
PLC print
Thermocouples set up Report
Thermocouples Qualification Report
All above documents are required for below attachments as per respective studies:
Attachment 06: For Heat Penetration Study for 20mm Rubber Stopper Minimum Load
Attachment 07: For Heat Penetration Study for Garment Sterilization Maximum Load
Attachment 8: For Heat Penetration Study for Garment Sterilization Minimum Load
Attachment 9: For Heat Penetration Study for Miscellaneous Load
9.0 Sampling Procedure:
Scan data at every 10 sec interval in Validator/Valprobe.

Minimum 10 nos. of temperature sensors placed in the chamber geometrically for temperature monitoring study.
Minimum 10 nos. of Biological Indicator placed in the chamber next to the temperature sensors for temperature monitoring study.
10.0 Acceptance Criteria:
10.1 Vacuum Leak Test
10.1.1The vacuum drop should not be more than 1mm Hg/ 1 min of vacuum hold.
10.2 Bowie-Dick Test:
10.2.1 The indicator paper / sheet should be uniform change in color (Brown) over the entire pattern of indicator sheet when compared with contro
10.3 Heat Distribution Study:
10.3.1Temperature distribution within the chamber must be between 121C to 123C at all location during the sterilization period (dwell time).
10.3.2There should not be any slowest heating point (Cold Spot) in the Autoclave chamber.
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10.3.3The equilibrium time should not be more than 30 sec.

10.4 Heat Penetration Study:
10.4.1Temperature distribution within the chamber must be between 121C to 123C at all location during the sterilization period (dwell time).
10.4.2Sterilization temperature should be maintained for NLT 15 min for minimum 10 thermocouple during hold period.
10.4.36-log reduction should be observed in any exposed biological indicators on complete incubation period.
10.4.4 The equilibrium time should not be more than 30 sec.
10.5 Action to be taken in case of failure:
10.5.1 If the vacuum leak test fail, this may be due to insertion of thermocouple, initiate the work request for the maintenance of autoclave leakage.
10.5.2If the Bowie-Dick test fails, this may be due to gasket leakage of leakage due to insertion of thermocouple. Initiate the work reques
maintenance leakage of autoclave.
10.5.3If the Heat penetration or Heat Distribution cycle fails in any respect, raised the deviation as per SOP. Discard the cycle, investigate the cause
failure. Make the required corrections / modifications by initiate the work request for the maintenance of equipment prior to carrying out three add
sterilization cycles.
10.5.4During the revalidation if any load configuration fails in any respect a deviation should log & load configuration should be invalidated. After
investigation, three runs of same load / modified load configuration to be validated with proper justification.
List of Standard Operating Procedure involved during validation study:
Sr.
SOP title
No.
1.
SOP No.
Issue No. / Revision

No.
Sterilization Procedure
Issue No. :
2.
Handling of biological Indicator
Rev. No.:
Issue No. :
3.
Operation of Kaye Validator 2000
Rev. No.:
Issue No. :
4.
Calibration of Measuring & testing

devices
5.
Operation of Val probe logger
Rev. No.:
Issue No. :
6.
Operation of HTR-400
Rev. No.:
Issue No. :
7.
Sterilization Procedure
Rev. No.:
Issue No. :
Rev. No.:
Issue No. :
Rev. No.:
Details of Equipment used for analysis

Sr.
Name of
Equipment
Equipment
No. / ID No.
No.
1.
2.
Last
Calibration /
Validation
done on
Next
Calibration /
Validation
due on
Remarks
Kaye Validator
2000
Val Probe logger
11.0 New risk observed if any During the process:
Pl. mention as it is report part

12.0 Discussion:
12.1 Procedure:To mention, how conducted the study.Pl. mention as it is report part
08/09/2016
12.2 Acceptance Criteria:Pl. mention as it is report part

12.3 Change Control Note:Study is conducted under any change control system , if yes, pl. mention.
12.4 Deviation:Pl. mention for deviation, if any.
12.5 Out of Specification:Pl. mention for OOS, if any.
12.6 Within Date:
12.6.1
Last Validation performed on : _________________
12.6.2
Current Validation performed on : _________________
Remarks (if any):

12.7 Training:Pl. mention about training details given for protocol execution to team members.
13.0 Modifications Suggested:
After execution of protocol, if any modification is suggested to get the desired results.
14.0 Conclusion:
Conclude the report for acceptance or non acceptance of equipment as per protocol acceptance criteria.
15.0 Records:
15.1 Standard Formats
Sr. No.
15.1.1
15.1.2
Format Detail
Records of All The Cycles/ Runs With Relevant Calculations
Bacterial Challenge Test Report For Heat Penetration Study
Document No.
15.2 Exhibits
Sr. No.
15.2.1
15.2.2
15.2.3
15.2.4
15.2.5
15.2.6
15.2.7
15.2.8
15.2.9
15.2.10
Exhibit Detail
Front View Of Sterilizer
Bowie-Dick Test Load
Temperature sensor distribution in Empty Chamber Heat
Distribution Cycle
Temperature sensor & BI distribution For 20mm Rubber
StopperMaximumLoad
Temperature sensor & BI distribution For 20mm Rubber
StopperMinimumLoad
Temperature sensor & BI distribution For32mmRubber
Stopper Maximum Load
Temperature sensor & BI distribution For32mmRubber
Stopper Minimum Load
Temperature sensor & BI distribution For Garment Maximum
Load
Temperature sensor & BI distribution For Garment Minimum
Load
Temperature sensor & BI distribution in Miscellaneous Load
Exhibit No.
Exhibit-X
Also see:Autoclave Validation in Pharmaceuticals

Ankur Choudhary is India's first professional pharmaceutical blogger, author and founder of Pharmaceutical Guidelines, a widely-read pharmac
blog since 2008. Sign-up for the free email updates for your daily dose of pharmaceutical tips.
Email: info@pharmaguideline.com. Need Help: Ask Question
08/09/2016

Process Performance Qual PDF

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Process Performance Qualification Protocol for Autoclave : Pharmaceutical Guidelines Page 1 of 13

Process Performance Qualification Protocol for Autoclave

Related:Low Temperature Sterilization Process (115C)

Memorandum 2010, Part 3 of 6,

Sterilization, June 2001

PDA Technical Monograph No. 1,

2005 Revision Supplement, Volume 59, Number X

Process Performance Qualification Protocol for Autoclave : Pharmaceutical Guidelines Page 2 of 13

To prepare/review standard operating procedure/protocol as per current

Review and approval of protocol and validation report.

Three (3) successful runs for all planned loads.

6.1.1 Empty chamber Heat Distribution:

Process Performance Qualification Protocol for Autoclave : Pharmaceutical Guidelines Page 3 of 13

Key operating parameters as per Operational Qualification identified are as below:

Pure Steam Pressure

6.3 Functional Risk Assessment

Process Performance Qualification Protocol for Autoclave : Pharmaceutical Guidelines Page 4 of 13

(S) Severity of Event (Consequence)

6.9 Detection of Adverse Event

(D) Level of Detection

6.11 Risk Review and Monitor Controls

6.12.1Nature of Risk & its mitigation action to the risk identified:

Process may gets

Only Qualified persons

Process may gets

System operation SOP

Process Performance Qualification Protocol for Autoclave : Pharmaceutical Guidelines Page 5 of 13

Fail is having indication

Result in Atypical cycle

May System loss

Load is not placed as

Load may not

Result in Atypical cycle

Chamber vacuum not

Process Performance Qualification Protocol for Autoclave : Pharmaceutical Guidelines Page 6 of 13

7.0 Equipments/ Material to be used for Validation Study:

Calibrated Valprobe loggers/Thermocouples

Process Performance Qualification Protocol for Autoclave : Pharmaceutical Guidelines Page 7 of 13

Loading tray constructed of Stainless steel SS316.

7.2.1TwoPT-100 probes, inserted in Chamber to monitor temperature on yokogawa recorder.

Vacuum leak test

Bowie Dick Cycle

Empty chamber Heat Distribution

Loaded chamber with Rubber

Heat Penetration study in Rubber closure RFS

7.4 Sterilization Cycle Parameters:

Select Cycle (Recipe No)

7.5 Recipe For Bowie Dick Cycle:

Select Cycle (Recipe No)

Initial vacuum time

Process Performance Qualification Protocol for Autoclave : Pharmaceutical Guidelines Page 8 of 13

Sterile Print Time

7.6 Recipe For HPHV RSD cycle:

Select Cycle (Recipe No)

Initial Vacuum Pulse

Initial Vacuum Value

Initial vacuum time

Sterile Hold Print Time

Dry Vacuum Pulse

Dry Vacuum Value

Dry Vacuum Time

JKT STM PRE REL