A validation programme involves various components in pharmaceutical organisation related to process, equipment and product.

1. EQUIPMENT VALIDATION :
HOT AIR OVEN
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Mr. Sagar Kishor Savale
[Department of Pharmaceutics]
avengersagar16@gmail.com
2015-2016
Department of Pharmacy (Pharmaceutics) | Sagar savale

2. Content
• Definition of Equipment validation
• Introduction
• Types of Dry Heat Sterilizers
• Principles of Heat Transfer And Circulation
• Validation Test Equipment
• Basic Validation Approach
• Process Qualification Cycle Development
• Routine Monitor After Validation
• Documentation
• Conclusion
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3. Introduction1,4,III
• A validation programme involves various components in
pharmaceutical organisation related to process, equipment and
product.
• Equipment Validation ensures that an instrument is appropriate for
its intended use.
• Dry heat is one of the most commonly used method to sterilize and
depyrogenate pharmaceutical components and product.
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4. Types of Dry Heat Sterilizers 1
Conventional Hot Air Oven
Tunnel Sterilizers
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5. HOT AIR OVEN 2,3,I
• Higher temperatures and longer exposure times required
• Typical cycles:
 160°C for 120 minutes
 170°C for 60 minutes
 180°C for 30 minutes
• Used for:
 glassware and product containers used in aseptic manufacture, non
aqueous thermostable powders and liquids (oils)
 also used for depyrogenation of glassware.
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6. The hot air oven is the equipment which is utilized to provide the dry heat
medium and it must be validated to ensure that the system is able to provides
sterile and depyrogenated components, on a reproducible basis
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7. Principles of Heat Transfer and Circulation 1,2,II
• Convection
 Heat flows from one body to another due to the temperature difference
between them.
• Radiation
 Photon propagation will transfer thermal energy to the object and increase
the surface temperature
• Circulation
 Booster fan or blowers are used in the oven to increase the circulation of
the heat throughout the load.
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8. Validation Test Equipment 1,IV
Equipment used for validation testing of oven are listed below:
 Resistance temperature detectors
 Thermocouples
 Data logger
 Constant temperature bath
 Stopwatch
 Voltmeter
 Optical tachometer
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9. Basic Validation Approach 3,4, V
Design qualification:
• The DQ outline the key features of the system designed to address
the user requirement, regulatory compliance and selection rationale
of a particular supplier.
• The following are the key considerations for DQ:
 Physical dimensions of the equipment and accessories
 Suitable operating environment of the instrument
 Health and safety requirement 95/29/2016

10. • It is carried out after or concurrently with the installation of the equipment at
the user’s premises.
• The purpose is to provide documentary evidence that the correct equipment
has been received and installed as per plan and protocol.
• IQ documents should be reviewed and approved by designated responsible
individuals.
• It includes details of-
 Structural- Check dimensions, presence of seal
 Filters- Proper identification,type,size,air capacity, flow rate
10
Installation Qualification
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 Electricals- Proper identification, safety cutoff
 HVAC- System provides the temperature and pressure differential required.
 Air supply- Identify source, duct size.
 Air or natural gas- Check that the source and type of supply are consistent
with the manufacturer’s recommendations.
 Heaters- Record the manufacturer's model no., the no. of heating elements.
 Blowers- Check for use of correct fan belt & that is in good condition.
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12. Operational Qualification
• It is documented verification that the system or subsystem performs as
intended throughout all specified operating range
.
• The OQ document should be reviewed and signed by the required
department representatives.
• The components of system must satisfy the operating ranges as determined
by the purchase order specifications.
• Each of the following process components must be identified & the
operating performance & range determined.
Temperature monitors
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 Cycle timer-
The accuracy of timer must be determined, so that assurance is
provided for cycle time.
 Door interlocks-
If a unit is equipped with double doors, the interlocks must operate
such that the door leading to the aseptic area cannot be opened if the
door to the non-aseptic area is opened.
 Heaters-
All of the heating elements must be functional.
 Blowers-
The air velocity consistent and motor speed of blowers should be
noted in the OQ records.
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 Cooling Coils-
If coils are present, the type and size of the coils and temperature of
the cooling medium at the inlet and outlet of the coils should be
recorded.
 Chamber leaks-
The perimeter of the doors for batch sterilizers should be checked for
air leakage while operating.
 Particulates counts-
Particulate count should be checked within the containers before and
after sterilization to quantitate the particle load contributed to the
product by sterilization process
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15. Performance Qualification 5
• Verifies that the equipment performs according to design specifications and
user defined requirements in a reliable & reproducible manner under
normal production conditions
• Physical -
Heat penetration studies on empty chamber
Heat distribution study on loaded chamber
Heat penetration study on loaded chamber
• Microbiological-
Bio-challenge/ Pyro-challenge studies
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16. Heat Penetration Studies On Empty Chamber 1,2,IV
• To identify heat distribution patterns including slowest heating points
• Multiple temperature sensing devices should be used(Thermocouples)
• Temperature profile locate hot/cold areas in the sterilizer by mapping
temperature at various locations
• A detailed diagram of the location of the thermocouples should be included
in the empty chamber data file
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17. Heat Distribution Study on Loaded Chamber1,2
• Multiple thermocouples throughout chamber (not inside product
containers) to determine effect of load configuration on temperature
distribution.
• Temperature distribution for all loads using all container sizes used in
production should be tested.
• Repeat runs should be performed to check variability.
• Temperature profile for each chamber load configuration should be
documented
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18. Heat Penetration Study on Loaded Chamber 1,2
• Designed to determine the location of the slowest heating point within a
oven at various locations.
• Each size & type of material should be tested by penetration studies.
• Hot areas in the load are more important for heat labile items.
• Data obtained by placing thermocouples inside the container in such a way
as to ensure contact with the surface.
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19. Bio-Challenge/ Pyro-Challenge Studies 1,2
• The challenge should demonstrate the lethality delivered by the cycle with
either microorganisms or endotoxin
• Resistant bacterial spores are available as BIs primarily in the form of:
• Spore strips:
• Spore suspension:
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20. Process Qualification Cycle Development 1,2,II
• The sterilization cycle is designed to inactivate the heat resistant spores as
well as any vegetative cells which could potentially be present during
processing.
• D-value:
 It is used to express the rate of killing of microorganisms during
sterilization.
 The time required at a certain temperature to kill 90% of the organism
being tested.
 Dry heat sterilization:Therotical requirment-170°C,32 min.
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• Z-value:
 The relationship of lethality to temperature is expressed the in Z-
value.
 The Z value will define the number of degrees that are required for a
change in the D-value by a factor of 10
 Dry heat sterilization Z =20°C
• F-value:
 It is a unit of lethality used as a measurement of sterilization
effectiveness.
 It indicates the equivalent amount of time delivered by a heat process at
a particular temperature.
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22. Routine Monitor After Validation 1,5
• The unit must be monitored so that it remains in a state of control
• This is achieved by the use of various programs including-
• Sanitization:
 It should detailed the cleaning methods used for the equipment, the
SOPs covering each method, and the cleaning materials utilized.
 Cleaning materials should be nontoxic and leave no residues.
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• Preventive maintenance-
 It provides a schedule by which the equipment is maintained.
 A proper PM program will help to prevent breakdown during
production.
• Change control-
 Changes to the equipment that might compromise the validation
must be brought to the attention of the group or individuals in
charge of the change control program.
• Revalidation-
 It may be required after changes or repairs are made on the unit or
an a predetermined periodic interval.
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24. Documentation 1,5
• All validation information should be easily identified and kept in a
permanent central file, where it can be readily retrieved.
• The validation file should include the following information:
• Qualifications-
This includes all steps performed in the certification of the equipment .
All original data, results and conclusion must be contained in this file.
All reports should be dated,signed,and approved by the responsible
individuals.
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• Process Qualification Protocol:
 The protocol is located in this file.
• Raw Data:
 All original data, results, calculation and conclusions must be retained for
empty- and loaded chamber and biochallenge studies
• Process Qualification Report:
 It is the formal document available for regulatory review
• Routine Monitoring:
 All change-control information and postvalidation mechanical changes are
recorded along with any revalidation work
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26. Conclusion
• Equipment is one of the basic component of pharma processing and
therefore equipment validation is an important aspect.
• Validation of Hot Air Oven is the part of comprehensive validation
program within a company.
• The validation of Hot Air Oven prove its repeatability.
• Equipment validation give the surety that equipment having good
qualification like design, operation, installation and performance
qualification which have predetermined.
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27. References
1. Laurie BC, Gayle DH, Dry Heat Sterilization and Depyrogenation
Validation and Monitoring, In:, James AF, Carleton J, Editors.Validation
Of Pharmaceutical Process, informa healthcare; P. 223-239
2. Michael JA,Neil RA. Sterilization Validation. In : Robert AN, Alfred HW,
Editors. Pharmaceutical Process Validation, New York: informa healthcare
; 2011 .P. 83-111
3. Gupta GD, Garg R, Aggarwal S. Guidlines On General Principles Of
Validation :Solid, Liquid and Sterile Dosage Forms, latest review, vol-
6(1),01/10/2008
4. Potdar AM. Pharmaceutical Quality Assurance,1st ed. Published by
Nirali Prakashan; 2006.P. 8.13-8.20
5. Syed Imtiaz Haider. Pharmaceutical Master Validation Plan. The Ultimate
Guide to FDA,GMP and GLP Compliance. informa healthcare;2010. P.
138-139
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28. Web References
I. http://www.mackpharmatech.com/doc.htm
II. http://www.radiantenergy.com/fin.htm
III. http://www.pharmainfo.net/equipment-validation-
articles/laboratory-equipment-qualification
IV. http://www.validation-online.net/validation-protocol-
standards.html
V. http://www.ehow.com/list_6809815_equipment-qualification-
protocols.html
VI. http://www.ikev.org/haber/2002validpdf/Sunum%20Suat%20Ku
mser.pdf
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