process performance qualification protocol for autoclave

7/30/2019 Process Performance Qualification Protocol for Autoclave

1/24

Process Performance Qualification Protocol for Autoclave

Validation Protocol of Autoclave (Steam Sterilizer) Sterilization Process i.e Autoclaving

Labels: fda process validation, fda process validation guidelines, gmp process validation, gmp validation process,manufacturing process validation, process validation guidelines, process validation in pharma

1.0 Objective:

The objective of this protocol is to verify the performance qualification attributes i.e. sterilization and toestablish sufficient data to assure that the STEAM 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 thelimit of 121 to 123C.

To ensure that the heat is sufficiently penetrating into the innermost portions of the load subjected forsterilization to achieve a temperature of 121C - 123C during the Sterilization hold period.

To ensure that the steam Sterilization process, when challenged with Geobacillus StereothermophilusBiological indicator spore strips having spore population of 106 spores strip, should reduce the bacterialload by more than 6 log.

2.0 Scope:

This Protocol shall be applicable to the Autoclave (Equipment No.: ABCD), situated in the cleanroom no. A10 in the HHHHH plant of ..Company, located atcity.

3.0 References:

3.1 Internal References

Sr. No. Reference Detail Document No.

01 Operation of KayeValidator

02 Calibration of Measuring & TestingDevices

03 Operation of HTR

04 Operation of Valprobe


2/24

loggers05 Handling of Biological

Indicator06 Risk Management07 Deviation

Management3.2 Others

Sr. No. Reference Detail Document No.

01 Scottish Health TechnicalMemorandum 2010, Part 3 of 6,Validation and verificationSterilization, June 2001

SHTM 2010

02 BRITISH STANDARD BS EN, Sterilization Steam sterilizers Large sterilizers (The European Standard EN 285: 1996)

EN 285

03 Industrial Moist Heat SterilizationIn AutoclavesPDA Technical Monograph No. 1,2005 Revision Supplement, Volume 59, Number X

PDA Journal of PharmaceuticalScience andTechnology

04 Sterilization of health care products Moist heat Part2: Guidance on the application of ANSI/AAMI/ISO 17665-1

ANSI/AAMI/ISO 17665-1

4.0 Responsibilities:

Department ResponsibilitiesQuality Assurance Q.A. Officer / Executive:

To prepare/review standard operatingprocedure/protocol as per current GMP requirement andorganizations Quality norms. To ensure & follow correct procedure written in SOP &protocol. Ensure the sampling instruction written in Protocol isfollowed to withdraw sample at specified location in specifiedtime interval and witness of validation activity. Test the collected product sample tested as perspecification. To report any abnormality to QA Manager / QA Head and

take corrective and preventive action in coordination withrespective department head.Q.A. Manager: Review & Approval of Protocol & Report. Ensure all the raw data generated were in accordancewith protocol & expected results achieved.Head - Q.A./ President-Technology:Review and approval of protocol and validation report.


3/24

Technical Department Executive / Manager Technical: Is responsible for review &scheduling the planned validation activity and to providetechnical support for execution of protocol.

Manufacturing Manufacturing Chemist: To follow instruction written in SOPProduction Manager/ Q.A. Manager Ensure implementation of BMR and protocol. Ensure the sample were withdrawn & sent to the QC fortesting as per specification. Ensure all the equipment used during Process validationwas 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 purgedout and the pressure in the chamber is maintained by further inlet of steam. Therefore uniform heatdistribution is expected in the steam sterilizer chamber during sterilization hold period and probabilityof non-uniformity within the chamber is less.

In the Autoclave steam inlet is from the both sides of the chamber through baffles, for uniformdistribution of steam in the chamber. Condensate drain point is located at the bottom. Three horizontalplanes of two shelves (i.e. top and bottom) are selected for temperature mapping. 4 probes to beplaced in four corners of top shelves, 3 probes at corner &1 probe at centre of top selves. 3 probes atcorner & 1 probe in drain point of lower shelves (attach layout)

6.1.2 Loaded chamber heat penetration:

For sterilization of Rubber stoppers, Garment & Miscellaneous Load (Silicone tube) the 5 probes areplaced inside the load, 1 probe in drain point and 4 probes in the chamber as per respective loadingpattern diagram attached as Exhibits to this protocol for monitoring of heat penetration in loadedchamber.


4/24

Once the maximum and minimum load are validated for Autoclave at defined validated Load patternneed not to qualify periodically for minimum load. Therefore only maximum loads will be periodicallyrevalidated 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 Process Parameter1 Pure Steam Pressure NLT 2.0 Bar (g)

2 Vacuum NLT 0.70 Bar (g)

3 Compressed Air 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 anddata integrity. It involves mainly following steps.

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 assessedagainst a series of GMP criteria.

Following types of risks are mainly identified during risk assessment process for qualification of systemas below:

Risks towards non-availability of required documentation

Risks towards non-availability of required SOPs

Risks towards non-availability of system Access Control


5/24

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 assessmentproceeds to identify the various risk scenarios i.e. the events that identify the risks associated with useof the system.

The functions identified are analyzed by considering possible hazards/adverse effects and what controlsmay be needed to minimize the potential harm.

6.6 Assessing the Likelihood of An Adverse Event

After identifying hazards / adverse events, determine the likelihood (frequency or probability) of itoccurring. User considers the likelihood of the adverse event occurring per number of transactions, andassigns 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 effectstake into account impact on regulatory compliance, impact on product quality and impact on dataintegrity.

The impact of risk occurring may be described as follows:

6.8 Ranking Of Adverse Event Severity

Table I

Value (S) Severity of Event (Consequence)3 High(H) : Can cause serious adverse

health consequences which canthreaten the life of Patient or evendeath

2 Medium(M) : Temporary or reversibleadverse health consequences but thelife of the patient is not threatened

1 Low(L) : No effect/Impact for patients


6/24

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 probability of detection, may not pose a serious threat because it can berecognized quickly and suitable corrective action taken to mitigate its impact. If an adverse event has a

low probability of detection, then the risk condition needs to seriously consider a review of the design orthe implementation of alternative procedures to avoid the event.

6.10 Ranking Of Adverse Event Detection

Table II

Value (D) Level of Detection1 High (H): The risk can be easily detected through deployed control measure/system and

the detection system is automated.

2 Medium (M): The risk can be detected later through deployed control measure/systemand the detection is through manual method

3 Low (L): The risk cannot be detected through deployed control measure/system thedetection 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. Periodic review after the system is fully operational /validatedshall

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:

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


7/24

Sr. No Descriptionof RiskIdentified

Impact Level of Riskaftermitigationplan (Low /Moderate /High)

Expectedresults

Observation

Tested By Sign & Date)Risk of System Access by Unauthorized/untrained personnel

1 Unauthorized person tries to conduct the process. Process may gets affected. Low Only Qualified persons are authorized to perform the process and conduct the study

2 Untrained operator tries to operate /maintenance of the system. Process may getsaffected. Low Training plan, training record and Operation SOP should be available.

3 Operation SOP does not contain proper information. Process may gets affected. Low System operation SOP should contain operation information as recommended by QA.

Risk on account of abnormal process condition occurred at the time of system operation

4 Failure of Vacuum leak test Process gets affected. Low Message appears on PLCLeak Test Fail.

SOP contains information to take action accordingly.


8/24

5 Failure of Bowie Dick Test Process gets affected. Low Fail is having indication of light color in center of pattern


6 Failure of Biological Indicator. Process gets affected. Low

Risk on account of abnormality in connected utilities at the time of system operation

8 If Pure steam pressure Low during running cycle. Process gets affected. Low Pressure and hence temperature not achieve in the system.

Result in Atypical cycle


9 Low vacuum Process gets affected. Low Result in Atypical cycle


10 Temperature lower during sterilization running the cycle. Process gets affected. Low

Temperature not achieve in the system.




9/24

11 Temperature higher during sterilization phase of cycle. May System loss or damage tocomponents Low Result in Atypical cycle


12 Load is not placed as per defined and validated load pattern Load may not get sterile Low SOP contains information to take action accordingly.

Authorized and trained person is performing the operation.

Risk occurred in Equipment

13 Door gaskets damaged Process gets affected. Low Chamber vacuum not maintained



14 Malfunctioning of pneumatic valves Process gets affected. Low Result in Atypicalcycle


15 Malfunctioning of Steam trap Process gets affected. Low Temperature not achievein the system




10/24

16 Failure of post calibration of thermocouple. Could not accessed about product sterilizationLow 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.

The Autoclave Chamber is made up of Stainless Steel sheet, which is welded with a U-Profile StainlessSteel Jacket. The Autoclave Chamber is provided with 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 pneumatic cylinder, when the door reaches the end position gaskets are pushed out automatically withhelp of compressed air for sealing similarly to open the door gasket is retracted by vacuum. When the


11/24

gasket is retracted the door slides automatically. The Door sealing is done with the help of tubular,silicone rubber gasket. To ensure proper sealing the gaskets are activated with compressed air andretracted 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 (non- sterile area side) and process lock to prevent opening of the door during the operation.

The Autoclave chamber is insulated with resin-bonded glass wool, which helps in reducing the heat lossto the environment and ensuring uniform distribution of temperature inside the chamber. Thisinsulation 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 between the Controlled area (Non-Sterile area side) and Clean area(Sterile area side), a Stainless steel flush paneling is provided on the partitioning wall and the outercover of Autoclave. All Joints, Crevices are filled with Silicon sealant to prevent any leakage.

The Autoclave is 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 thesterilization chamber for smooth and easy operation of the load article.

Loading tray constructed of Stainless steel SS316.

Chamber Compound gauge on sterile and Controlled area side, Jacket pressure gauge of theControlled area side, Gasket compound gauge for both the doors on the Controlled area side and criticalarea 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 generationroom.

Control panel consisting of PLC, Digital Temperature input to the microproce ssor from a 5 Nos of Temperature transmitters, one Pressure transmitter, Pressure and vacuum switches for giving digitalpressure/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 solenoidvalves to regulate air supply to the pneumatic rotary actuators.

7.2 Monitoring and Controlling of the sterilization cycle:

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

7.2.2 One 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 yokogawa recorder.


12/24

7.3 Study Design:

S. No.

Study Name of the Recipe No. of trials tobe taken

Vacuum leak test Leak Test One

Bowie Dick Cycle Bowie-Dick One

Empty chamber HeatDistribution

HPHV RSD One

Loaded chamber withRubber Stoppers

HPHV RSD One

Loaded chamber withgarment and handgloves

HPHV RSD One

Loaded chamber withMiscellaneous items(Silicone tube)

HPHV RSD One

Note: - New load may be introduce in loading pattern in between two scheduled re- qualification studyafter three successful validation run and report of same shall be attached as addendum to last validationreport.*

Reference cycle detail (Initial validation with Protocol No)

Sr. No. Protocol No. Protocol No.1 Heat Penetration study in

Rubber closure RFS (Ready ForSterilization) bag (Applicable for20 mm rubber stopper)

2 Heat Penetration study forGarment Sterilization

3 Heat Penetration study forMiscellaneous Load

7.4 Sterilization Cycle Parameters:

Sr.No

Name of Parameter Leak test

1 Programme Name Vacuum Leak Test2 Select Cycle (Recipe No) 43 Leak Vacuum on -0.7 kg/cm24 Vacuum Hold 15 min


13/24

7.5 Recipe For Bowie Dick Cycle:

7.6 Recipe For HPHV RSD cycle:

Sr. No Name of Parameter Value

1. Select Cycle (Recipe No) 7

2. Initial Vacuum Pulse 3

3. Initial Vacuum Value 500 mm of Hg

4. Initial vacuum time 2 min

5. Preheating Temperature 95 C

6. Preheating Time 1 min

7. Sterile Temperature 121.0 C

8. Sterile Time 15 min

9. Sterile Hold Print Time 60 sec

10. Dry Vacuum Pulse 3

11. Dry Vacuum Value 600 mm of Hg

12. Dry Vacuum Time 20 min

Sr. No Name of Parameter Bowie Dick Test

1 Select Cycle (Recipe No) 5

2 Initial vacuum time 2 min3 Pulsation 34 Preheating Temperature 95C

5 Preheating Time 1 min6 Sterile Temperature 121.0 C7 Sterile Time 10 min8 Sterile Print Time 1 min

9 Dry Vacuum Time 0 min10 Dry Vacuum Value -0.700 Kg/cm211 Door Open Temperature 90 deg


14/24

13. JKT STM PRE REL 2 min

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

8.0 Procedure:

8.1 Vacuum leak test Procedure:

8.1.1 Put the flexible probes inside the chamber through the validation port provided for the validationcycles prior to start of Vacuum leak test.

8.1.2 Ensure that Autoclave is empty and chamber is at ambient temperature.

8.1.3 Ensure compressed air is ON at required pressure of 6 bar.

8.1.4 Ensure sufficient water supply is available for seal of vacuum pump

8.1.5 Ensure gasket lubrication is proper

8.1.6 Switch ON Main switch provided on panel board.

8.1.7 Close 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.

8.1.9 Check the programme from control panel.

8.1.10 Enter the Operator level password & enter the programme as per requirement.

8.1.11 Select programme by pressing Enter Key F1 once.

8.1.12 All parameter will start on displaying on screen one by one.

8.1.13 Enter F1 button and select programme, the display will show YES-1 NO-2.

8.1.14 Checks the online printer attached to PLC & then select 1 and press Enter.


15/24

8.1.15 Cycle will start in automatic m ode as per set parameter as PLC will show Leak Test Vac ON andvacuum will be created in chamber.

8.1.16 After completion of hold period, vacuum release valve will open and message will display LeakTest Vac Release and continue till the chamber press ure comes to atmospheric pressure.

8.1.17 At the end of the cycle, if the leak rate is more than 1 mm of Hg/ min during hold period, thenmessage will display Leak Test Fail & if it is less than 1 mm of Hg/min during hold period, thenmessage will displ ay Leak Test Pass.

8.1.18 If cycle fails, initiate work request form for rectification of problem.

8.1.19 After rectification of problem fresh cycle to be run. Upon completion of cycle screen will displayCycle Over.

8.1.20 Continue to run for next cycle of Bowie-Dick test.

8.2 Bowie Dick test Procedure:

8.2.1 Load the tray in the autoclave chamber.

8.2.2 Place the Bowie-Dick test pack on the bottom shelf of the sterilizer just above the drain point(Nearly 100 mm over the drain).

8.2.3 Selected 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 minutes, at 121C. (Manufacturers recommendation).

8.2.4 Start the cycle by pressing Enter key.

8.2.5 After the cycle is over, open the door from control area side & take the sterilized test pack fromthe Autoclave and check the indicator paper/strip for uniform color change.

8.2.6 Observation should be recorded in test data sheet no 05 (Exhibit II).

8.2.7 A Fail is indicated by light color in the center of the pattern than around the edges whencompared with control.

8.2.8 Failure of the pattern to change completely black or dark brown at 121 C when compared withcontrol.

8.3 Procedure For Empty Chamber Heat Distribution Study

8.3.1 Connect the calibrated thermocouples with SIM to the Kaye Validator and distribute thesethermocouple through out chamber as per Exhibit-III.

8.3.2 Operate Kaye Validator as per SOP or Val probe logger as per SOP.

8.3.3 Run HPHV RSD cycle as per SOP with recipe defined in point 7.6.


16/24

8.3.4 Select the cycle from the MMI/ HMI panel as per point no.8.1.10 to 8.1.12 & start HPHV RSD cycleas well as start Kaye Validator at same time. Scan data at every 10 sec interval in Validator.

8.3.5 After completion of the cycle take the printout of report generated through Kaye Validator.Evaluate the report as per acceptance criteria.

8.3.6 Attach the report generated through Kaye Validator and PLC print out & graph from chart lessrecorder to the report.

8.4 HEAT PENETRATION STUDIES

8.4.1 Procedure For Loaded chamber heat penetration study:

8.4.1.1 Load the articles into Double door Autoclave as per their respective loading diagram attached asexhibit to this protocol.

8.4.1.2 Place heat penetration probes inside the loaded articles and select the positions where heat

penetration is difficult.

8.4.1.3 Connect the Thermocouple with SIM to Kaye Validator as per SOP or Val probe logger as perSOP, which senses the temperature.

8.4.1.4 Place biological indicator folded with aluminum foil strips of Geobacillus Stereothermophiluscontaining 106 spores along with flexible probes.

8.4.1.5 Select the HPHV RSD cycle as per point no. 8.1.10 to 8.1.12.

8.4.1.6 Start 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 interval in Validator.

8.4.1.7 After completion of the cycle take the printout of report generated through Kaye Validator.Evaluate the report as per acceptance criteria

8.4.1.8 Carry out total three replicate runs with loaded chamber for newly introduced load (first timestudy).

8.4.1.9 Take out all exposed biological indicator strips & send the biological indicator to microbiologicallab for testing as per SOP and recording the results in observation sheet.

8.4.2 Heat Penetration Study: Maximum Load of 20mm Rubber Stopper in RFS Bag (Ready ForSterilization)

8.4.2.1 Load 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 ready for sterilization in the chamber of autoclave in two trays asper defined loading diagram attached with this protocol.

8.4.3 Heat Penetration Study: Minimum Load of 20mm Rubber Stopper in RFS Bag


17/24

8.4.3.1 Load the 20 mm rubber stopper (2500 nos. x 1 bags = 2,500 nos.) packed in Rexam pack readyfor sterilization in the chamber of autoclave in two trays as per defined loading diagram attached withthis protocol.

8.4.4 Heat Penetration Study: Garment Sterilization with Maximum Load

8.4.4.1 Load the 32 numbers of garment packed in baby bag & 32 goggle for sterilization in the chamberof autoclave in two trays as per defined loading diagram attached (Exhibit VIII) with this protocol.

8.5 Heat Penetration Study: Garment Sterilization with Minimum Load

8.5.1 Load the 5 numbers of garment packed in baby bag & 5 goggle for sterilization in the chamber of autoclave in two trays as per defined loading diagram attached (Exhibit IX) with this protocol.

8.6 Heat Penetration Study: Miscellaneous Load (Silicone Tube)

8.6.1 Ensure cleaning of Silicone tube before packing in Rexam bag.

8.6.2 Keep the silicone pipe (Approx 2 meter long) in Rexam bag by folding in circular way, keeping bothend open.

8.6.3 Insert the biological Indicator folded with aluminum foil along with Thermocouple in both end of silicone tube. Insert the probe as long as it goes inside the tube. Care should be taken when insertionthat after sterilization the biological indicator should be removed easily.

8.6.4 Load the 4 number of silicone tube packed in Rexam pack ready for sterilization in the chamber of autoclave in two trays as per defined loading diagram attached with this protocol.

8.7 Load Configuration:

Sr. No Load No Name of the Load Load Pattern Load Type No of Articles

01 NA Leak Test NA NA NA

02 NA Bowie Dick Test Bowie Dick NA 1 No

03 1 Rubber Stopper 20 mm Rubber Stopper

(5000 nos x 05 bags)

or (2500 nos x 10 bags) Maximum 25,000 Nos

04 3 Rubber Stopper 20 mm Rubber Stopper

(2500 nos x 1 bag) Minimum 2,500 Nos

05


18/24

10 Garment Load Garment Bags Maximum 32

Goggle 32

06 11 Garment Load Garment Bags Minimum 5

Goggle 5

07 12 Miscellaneous Load Silicon tube NA 4

Note:

1. During validation study, if there is any change required in the type and/ number of articles to beloaded, loading diagram will be changed. As per the validation result the diagrams will be established forroutine cycles and accordingly SOP will be established. In this case protocol will not be revised, as

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

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


19/24

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 temperaturemonitoring study.

Minimum 10 nos. of Biological Indicator placed in the chamber next to the temperature sensors fortemperature monitoring study.

10.0 Acceptance Criteria:

10.1 Vacuum Leak Test

10.1.1 The 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 control.

10.3 Heat Distribution Study:


20/24

10.3.1 Temperature distribution within the chamber must be between 121C to 123C at all locationduring the sterilization period (dwell time).

10.3.2 There should not be any slowest heating point (Cold Spot) in the Autoclave chamber.

10.3.3 The equilibrium time should not be more than 30 sec.

10.4 Heat Penetration Study:

10.4.1 Temperature distribution within the chamber must be between 121C to 123C at all locationduring the sterilization period (dwell time).

10.4.2 Sterilization temperature should be maintained for NLT 15 min for minimum 10 thermocoupleduring hold period.

10.4.3 6-log reduction should be observed in any exposed biological indicators on complete incubationperiod.

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.

10.5.2 If the Bowie-Dick test fails, this may be due to gasket leakage of leakage due to insertion of thermocouple. Initiate the work request for the maintenance leakage of autoclave.

10.5.3 If the Heat penetration or Heat Distribution cycle fails in any respect, raised the deviation as perSOP. Discard the cycle, investigate the cause of failure. Make the required corrections / modifications byinitiate the work request for the maintenance of equipment prior to carrying out three additionalsterilization cycles.

10.5.4 During the revalidation if any load configuration fails in any respect a deviation should log & loadconfiguration should be invalidated. After through 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.

No. SOP title SOP No. Issue No. / Revision No.


21/24

1. Sterilization Procedure

Issue No. :

Rev. No. :

2. Handling of biological Indicator

Issue No. :

Rev. No. :

3. Operation of Kaye Validator 2000

Issue No. :

Rev. No. :

4. Calibration of Measuring & testing devices

Issue No. :

Rev. No. :

5. Operation of Val probe logger

Issue No. :

Rev. No. :

6. Operation of HTR-400

Issue No. :

Rev. No. :

7. Sterilization Procedure

Issue No. :

Rev. No. :

Details of Equipment used for analysisSr.


22/24

No. Name of Equipment Equipment No. / ID No. Last Calibration / Validation done on NextCalibration / Validation due on Remarks

1. Kaye Validator 2000

2. 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

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.


23/24


24/24

15.2.8 Temperature sensor & BI distribution For Garment Maximum Load

15.2.9 Temperature sensor & BI distribution For Garment Minimum Load

15.2.10 Temperature sensor & BI distribution in Miscellaneous Load Exhibit-X

process performance qualification protocol for autoclave

Documents