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Compressed Air Validation Protocol

Compressed air validation is recorded evidence that such parameters as aerosol particle content, dew point, liquid water concentration, vapor content, oil aerosols, and other pollutants are within limits and do not cause product contamination.

Validation of Compressed Air

1.0   Objective

    • The purpose of this protocol is to provide the procedure for the Validation of compressed air distribution system
    • The system is capable of performing as specified in acceptance criteria, when operated in prescribe manner.
    • The adequacy of the engineering design of the equipment and the effectiveness of the operating control and maintenance procedures

2.0    Scope

    • This protocol covers all aspects of Validation for Compressed air Distribution system.

3.0   Reference Document for Compressed Air Validation

    • Following documents are referred during preparation of the compressed air validation protocol.
Document Name Document Number
Operational Qualification Protocol
SOP on Operation and maintenance of Air borne Particle counter
Operational SOP for air sampler

4.0   Equipment Description

    • Compressed air distribution system is used to provide compressed air with Control over moisture, microorganisms and oil as appropriate for the manufacturing and processing of drug products. Compressed Air filtration systems are used where appropriate on Compressed Air supplies to designated production areas .
    • It should be maintained the minimum _____kg/cm2 at the use point. Compressed air distribution pipe line connected from the main compressed air line after air dryer.
    • After that collect in air receiver, And Filtered by hydrophobic cartridge filter 40µ, 10µ, 1µ, 0.2µ and supply to the user point.

5.0   Responsibility – Compressed Air Validation

    • Responsibilities of different department/ personnel involved in different activities related to the Validation of for Compressed air distribution system are defined below:
    • Quality Assurance (Validation)
    • Preparation and review of Validation protocol.
    • Approval of Validation protocol.
    • Execution of Validation protocol along with the co-ordination of other departments.
    • Review of results and compiling of reports.Compressed Air Validation Protocol
    • Preparation and approval of Validation report.
    • Production
    • Checking of Validation protocol and Report.
    • Execution of Validation protocol along with QA validation team.
    • Engineering
    • Preventive Maintenance as per schedule.
    • Rectification of Breakdown during qualification study.
    • Quality Control
    • Performing Compressed Air Microbial and Sterility sampling and testing.
    • Performing Air borne Particle count.
    • Checking of Validation protocol and report.
    • Performing Compressed Air sample testing for Moisture and Oil
    • Preparation of analysis report and submission to Quality Assurance

6.0   Compressed Air Validation Test Method

    • Pre-Requisites

    • Prior to conducting/ executing the Validation protocol following conditions must be fulfilled:
    • System should be safe for execution.
    • Approval of Operational Qualification report.
    • All utilities shall be available.

    • Pre-Qualification test

    • Verification of Calibration of all measuring instruments of machine.
    • Calibration Verification of  all test instruments.
    • Verification of Standard operating procedure status.
    • Verification of Integrity test of air filters in line and at user points.

    • Validation Test Program

    • Moisture and oil testing.
    • Non- Viable particulate count.
    • Microbiological monitoring.
    • Test for total aerobic microbial counts.

    • Test Matrix

    • Following matrix shall be followed for the initial qualification and re-qualification Compressed air Distribution system for its performance:
Sr. No. Test Frequency Other Requirement
Initial Qualification Re –

Qualification
A.     Pre – Qualification Test
1 Verification of Calibration status of Measuring Instruments Once Once NA
2 Verification of Calibration status of test instrument. Once Once NA
3 Verification  of SOP status Once Once NA
4 Verification of Integrity Test at user point. Once Once NA
B.     Qualification Test
1 Oil Content Tester 03 days 01 day The test can be done by external vendor or In-house.
2 Non Viable Particle Count 03 days 01 day NA
3 Aerobic Microbial Count 03 days 01 day NA

 7.0   Procedure of Compressed Air Validation

    • Pre-qualification test procedure

    • Verification of Calibration status of measuring instruments

    • Objective:
    • To verify that all measuring instruments used in the equipment are in calibrated condition prior to execute the performance test.
    • Test Procedure:
    • Verify the calibration status of all the measuring instruments available on the equipment from the calibration certificate available
    • Acceptance criteria:
    • All measuring instruments shall be in calibrated status.
    • Observations and Results:
    • Record the observations and results in the format enclosed as Annexure 01.

    • Verification of Calibration Status of Test Instruments

    • Objective:
    • To verify that all test instruments used in the equipment qualification activity are in calibrated condition prior to test execution
    • Test Procedure:
    • Verify the calibration status of all the test instruments to be used during Validation study from the calibration certificate available.
Sr. No. Test Instrument Description
1 Oil content tester
2 Particle count tester
3 Instrument for microbial limit testing
    • Acceptance Criteria:
    • All test instruments shall be in calibrated status.
    • Observations and Results:
    • Record the observations and results in the format enclosed as Annexure 02.

    • Verification of SOP status

    • Objective:
    • To verify that the current version of SOP shall be used during Validation study.
    • Test Procedure:
    • Verify that the current version of SOP shall be used during Validation study by reviewing SOP.
Sr. No. SOP Title SOP No.
1 SOP on Operation and maintenance of Air borne Particle counter
2 Operational SOP for air sampler
    • Acceptance Criteria:
    • All SOP shall be available in current version.
    • Observations and Results:
    • Record the observations and results in the format enclosed as Annexure 03.

    • Verification of Integrity Test of Air filters at user points

    • Objective:
    • To verify that the integrity test of Air filters in distribution line and at user points has been done and all filters are passing the integrity test.
    • Test Procedure:
    • Verify the integrity test record of the Air filters.
    • Acceptance Criteria:
    • All air filters are integrity tested and passing the test.
    • Observations and Results:
    • Record the observations and results in the format enclosed as Annexure 04.

    • Moisture and Oil Monitoring

    • Objective:

    • The objective of this test is to show that the Moisture and Oil content are within defined values and Odor characteristic meet the requirements
    • Test Requirements:
    • System in operation.
    • Gastec tube
    • Test Procedure:
    • This test shall be performed by the external testing laboratory as per protocol
    • This test can be done in house also by using Gastec tubes.(addendum No.01 to
    • Protocol VD/ or by using gas detector tubes (Gastec).
    • Acceptance Criteria:

Oil: ≤ 0.5 mg/m3

Moisture: ≤ 0.5 g/m3

    • Observations and Results:
    • Record the observations and results in the format enclosed as Annexure 05.
    • Scientific rationale:
    • The limit is given as per in house specification of compressed air.

    • Non-Viable Particulate Count

    • Objective
    • The objective of this test is to prove that the non-viable particulate count is within the specification.
    • Connect the user point to a SS box (with inlet and out let) to diffuse the high pressure of air/gas to appropriate pressure to enable counting. Slowly open the user point and allow some air/gas to flush the box.
    • Place the sampling probe of the particle counter at the out let of the SS box and sample for 1-cubic feet of air or volume.
    • Take the print of the particle counter and record results.
    • Acceptance Criteria: shall comply for room classification limits as follows:
Grade Particles/ft3
≥0.5µ ≥5.0µ
Grade A 100 1
              Grade B 100 1
              Grade C 10000 57
              Grade D 100000 571
Other Grade (Grade E,O,etc) For Information
    • Results
    • Record the observation in the data sheet attached as Annexure-6.
    • Scientific rationale:
    • The limit is given as per in house specification of compressed air.

    • Aerobic Microbial Count

    • Objective
    • The objective of this test is to verify that the Compressed Air Distribution System can provide the required cleanliness with respect to microbiological contamination as defined in Standards.

    • Test for Total Aerobic Microbial Counts

    • Transfer the pre incubated Soybean Casein Digest Agar cassette, M Air T CG Sampler and accessories to the area to be monitored in a closed container to avoid any contamination.
    • Write the sampling location ID and date of sampling on the base of cassette
    • Connect the sampling point to M Air T CG Sampler to and perform sampling for 1000 litres.
    • After completion of air sampling close the cassette with lid.
    • Collect all exposed cassette in a closed container and transfer the plates to incubators for incubation.
    • Incubate the exposed cassettes along with negative control in inverted position at 30-35oC for 5 Days.
    • After incubation observe and count the number of colonies and record the results.
    • Acceptance Criteria: Shall Comply for Room Classification Limits as follows:
Grade Action Limit CFU/m3
Grade A 1
Grade B 10
Grade C 100
Grade D 200
Other Grades (Grade E, O, etc) For Information
    • Record the observation in the data sheet attached as Annexure-7.
    • Scientific rationale:
    • The limit is given as per in house specification of compressed air.
    • Sampling Matrix
    • Validation Study (3 Days)
  Sample code

(Location ID.)

 Sample Point Moisture, Oil and Odor Non Viable Counts Microbial

Monitoring

 Grade

    • Re qualification And Action To be Taken In Case Of Failure

    • Performance re-qualification of Compressed air Distribution system will be performed every year as per the test matrix mentioned in the protocol.
    • The qualification should also be performed additionally in case of following:
    • Any major modification in equipment after the last Validation. This must be properly documented through a change control system.
    • Any change in operational parameters with respect to that specified.
    • Any other factors based on Risk Assessment.
    • In case of failure to meet acceptance criteria of any test as mentioned in the protocol a thorough investigation is to be initiated to find out the root cause and the complete study or a part of the study may be repeated after the corrective action based on a suitable Risk Assessment of the Situation. However, if the failure is due to some obvious reason like power failure during the runs then the  affected run may aborted and repeat run shall initiated but the aborted run result along with description of the incident must be reported in the Validation report.

9.0   Documentation of Compressed Air Validation Study

    • Results and reports shall be compiled in a binder. Binder shall contain the following sequentially
    • Summary Report
    • Validation Protocol
    • Test Reports
    • Summary report shall be in narrative form, which describes the work as well as conclusion/certification regarding acceptability. Summary Report shall contain the following
    • Post Approval
    • Objective
    • Acceptance criteria
    • Brief validation methodology
    • Evaluation of results
    • Final result summary
    • Deviation, failure investigation reports and corrective actions (if any)
    • Conclusion

10.0        Conclusion

    • Based on the review of results a conclusion shall be drawn and documented in the summary report. Conclusion shall be a clear statement of compliance or noncompliance of the Compressed air Distribution system with respect to the acceptance criteria of the Validation protocol.

11.0        Abbreviations

Abbreviations Full Form
CFU Colony Forming Unit
VD Validation Documents
SOP Standard Operating Procedure
No. Number
µ Micron
°C Degree Centigrade
LPC Liquid particle counter
NMT Not more than

 

Annexure 1 : Calibration status of measuring Instrument Datasheet

Equipment detail:

Equipment
Equipment ID
Room ID
Area Location
Area Classification

 Measuring Instrument Details:

Acceptance Criteria Instrument should be in calibrated period
Instrument Name
Make
Instrument ID
Calibration Date
Calibration Due Date
Calibration Certificate Attached

 

Annexure 2 : Calibration status of Test Instrument Datasheet

Equipment detail:

Equipment
Equipment ID
Room ID
Area Location
Area Classification

 Test Instrument Details:

Test Date:
Acceptance Criteria Instrument should be in calibrated period
Instrument Name
Make
Instrument ID
Calibration Date
Calibration Due Date
Calibration Certificate Attached

 Remarks:

Annexure 3 : SOP Verification

Equipment detail:

Equipment: Compressed Air Distribution System
Equipment Location

SOP Verification:

SOP NAME  SOP Number  Revision No     Effective date
 
 
 

Annexure 4 : Integrity Test

Equipment detail:

Equipment: Compressed Air Distribution System
Equipment Location Service floor and Process area Lyo-Expansion

 

Vent Filter Integrity Test Details:

Air Filter Location Integrity test Done(Yes/No) Result  (Pass/Fail) Date of Testing
 
 
 

Annexure 5 : Oil and Moisture Content

Date of sampling Sampler I.D
 Sampled Volume Sampled by

Results:

S. No. Sampling Location ID Oil and moisture content            Remarks
1.
2
3
  • Acceptance Criteria:

Oil: ≤ 0.5 mg/m3

Moisture:≤0.5 g/m3

 Remarks:     The Results are with in the limits / not within the limits.

Annexure 6 : Non -Viable Particle count

Date of sampling Sampler I.D
Vol. of air sampled Sampled by

Results:

S. No. Sampling Location ID Grade Particles Remarks
³ 0.5 m / ft3 ³ 5 m / ft3
1.
2
3
4
5

Acceptance Criteria:

S. No. Grade Particles
 0.5 m³ / ft3
01 Grade-A 100
02 Grade-B 100
03 Grade-C 10000
04 Grade-D 100000
05 Other Classes (Grade E, O,etc) For Information only

Remarks:     The Results are with in the limits / not within the limits.

Annexure 7 : Total Aerobic Microbial Count

Date of sampling Air sampler I.D Incubation Temp. 32.5 ± 2.5°C
Media Lot No Vol. of air sampled Incubator ID
Use before date Start date
Date of Release Sampled by End date

Incubation Condition: 32.5 ± 2.5°C for 5 days

Results:

S. No. Sampling Location ID Grade Observation   (CFU/Plate/m3)  Remarks
Bacteria Fungi
1.
2
3
4
5

 

 

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Janki Singh is experienced in Pharmaceuticals, author and founder of Pharma Beginners, an ultimate pharmaceutical blogging platform. Email: [email protected]

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