CELEBRITY BIOPHARMA LIMITED

Format No.: QAS001/F/01/00 Reference SOP No.: SOP/QA/001/00

STANDARD OPERATING PROCEDURE
Location Quality Assurance SOP Number SOP/QA/038/00
Version 00
Superseded SOP No. Nil
Title Process Validation Effective Date
Review Date
Page Number 1 of 9

1. OBJECTIVE
1.1 To establish a procedure and guideline for process validation activity.
2. SCOPE
2.1 This procedure is applicable to process Validation of all products manufactured at Celebrity
Biopharma Limited.
3. RESPONSIBILITY
3.1 Quality Assurance Team: preparation of Protocol and Report. Sampling, Execution,
verification compilation of final report and approval of validation programme.
3.2 Production Team: checking of protocol and report. Execution of process validation as per
the approved protocol.
3.3 Quality Control Team: To analyze in process samples and preparation of analysis report.
3.4 Engineering Team: To provide technical support during validation activity.
4. PROCEDURE
4.1 Definition:
4.1.1 Process Validation:
A documented evidence to prove that a specific process, when carried out within
defined parameters will consistently produce an end product meeting its
predetermined specifications.
4.2 Types of Process Validation:
4.2.1 Process Validation can be categorizes as Prospective, Concurrent, Retrospective
and Revalidation.
4.2.1.1 Prospective Validation is carried out during the development stage on
the lab scale or pilot scale batches of the products that are under pipeline

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 CELEBRITY BIOPHARMA LIMITED
Format No.: QAS001/F/01/00 Reference SOP No.: SOP/QA/001/00
STANDARD OPERATING PROCEDURE
Location Quality Assurance SOP Number SOP/QA/038/00
Version 00
Superseded SOP No. Nil
Title Process Validation Effective Date
Review Date
Page Number 2 of 9

to be manufactured on a large scale.

4.2.1.2 Concurrent Validation is carried out during normal production;
Concurrent validation is done upon introduction of a New Product,
Change in Master Formula, Change in Process, Change in Equipment,
and Change in Location of Manufacturing.
4.2.1.3 Retrospective Validation involves the examination of past experience
of production on the assumption that composition, procedures, and
equipment remains unchanged; such experience and the result of in-
process and final control tests are then evaluated.
4.3 Process Validation Policy:
4.3.1 Process Validation shall be carried out for the following reasons:
4.3.1.1 A new product is manufactured in the facility.
4.3.1.2 An existing product is transferred from one manufacturing location to
another.
4.3.1.3 Changes of raw materials (physical properties such as density, viscosity,
particle size distribution may affect the process or product).
4.3.1.4 Change in existing formula or process.
4.3.1.5 Change in equipment, which has a direct impact on the manufacturing
process.
4.3.1.6 In case of different batch size of similar product, maximum and
minimum batch size shall validate.
4.3.1.7 Change in Production area (areas with equipments of different make /
capacity / working principle) and major changes in the support system as
identified by the validation committee members.
4.3.1.8 As per the Regulatory body requirement.
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 CELEBRITY BIOPHARMA LIMITED
Format No.: QAS001/F/01/00 Reference SOP No.: SOP/QA/001/00
STANDARD OPERATING PROCEDURE
Location Quality Assurance SOP Number SOP/QA/038/00
Version 00
Superseded SOP No. Nil
Title Process Validation Effective Date
Review Date
Page Number 3 of 9

4.3.2 Validation Procedure:

4.3.2.1 Based on company’s decision to introduce a new product or based on the
work order and considering the availability of raw & packing material,
production will be planned.
4.3.2.2 Initial checks for Process Validation:
4.3.2.2.1 All equipments used for validation programme must be
Qualified and wherever necessary calibrated and verified.
4.3.2.2.2 Availability of approved process validation protocol.
4.3.2.2.3 All Analytical methods used for testing of the product have
been validated.
4.3.2.2.4 All related Master Documents like: MFR, BMR, BPR and
FPS are available.
4.3.2.2.5 All SOP’s related to the validation programme are available.
4.3.2.2.6 Trained personnel shall carryout the validation.
4.3.2.2.7 All the Raw materials and Primary Packing Materials are
Tested and Released by quality control.
4.3.2.3 Process validation protocol shall include manufacturing flow chart with
detailed description of manufacturing procedure, drawing of sampling
plan with respect to equipment involved during the process, in process
test to be performed and its acceptance criteria. The process validation
protocol shall also include the critical parameters identified based on the
initial formulation which shall be optimized and validated.

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 CELEBRITY BIOPHARMA LIMITED
Format No.: QAS001/F/01/00 Reference SOP No.: SOP/QA/001/00
STANDARD OPERATING PROCEDURE
Location Quality Assurance SOP Number SOP/QA/038/00
Version 00
Superseded SOP No. Nil
Title Process Validation Effective Date
Review Date
Page Number 4 of 9

4.3.2.4 Quality assurance representative in consultation with Head production /

Regulatory /Head quality assurance will prepare the process validation
Protocol and report.
4.3.2.5 The Header comprises of
4.3.2.5.1 Company Logo on Right top corner of page.
4.3.2.5.2 Process Validation Protocol
4.3.2.5.3 Section: General Block /Beta Lactam Block
4.3.2.5.4 PVP Number: (The PVP No. is assigned by quality
assurance)
4.3.2.5.5 Product Name: (As per name mentioned in the MFR/BMR of
the product)
4.3.2.5.6 Generic Name: Generic name of product.
4.3.2.5.7 Effective Date: (Written in blue ink by quality assurance
after finalization of document)
4.3.2.5.8 Product Code: Product Code of product.
4.3.2.5.9 Page No.: X of Y.
4.3.2.6 The footer on first page comprises of Signatures of Prepared By (Quality
assurance), Checked By (Production, Quality Control), and Approved
By (Quality Assurance).
4.3.2.7 Note-for Process validation report header and footer same as mention in
pint no- 4.3.2.5 and 4.3.2.6, only PVP to be replaced by PVR.
4.3.2.8 The Quality Assurance Department assigns tracking number to PVP and
PVR as per procedure for ‘Master Document Numbering System’, SOP
No. SOP/QA/042.

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 CELEBRITY BIOPHARMA LIMITED
Format No.: QAS001/F/01/00 Reference SOP No.: SOP/QA/001/00
STANDARD OPERATING PROCEDURE
Location Quality Assurance SOP Number SOP/QA/038/00
Version 00
Superseded SOP No. Nil
Title Process Validation Effective Date
Review Date
Page Number 5 of 9

4.3.2.1 The protocol will be reviewed and Authorized by Production, quality

0 control and quality assurance personnel.
4.3.2.1 Upon receiving BMR request, quality assurance will issue a controlled
1 copy of BMR and the validation protocol for the said product.
4.3.2.1 Material will be dispensed as per quantities given in BMR and validation
2 protocol.
4.3.2.1 Dispensed material is then taking for further manufacturing processes.
3
4.3.2.1 The manufacturing process will be carried out stepwise.
4
4.3.2.1 As per protocol, quality assurance officer will keep ready required
5 sampling bags, identification labels and sampling tools.
4.3.2.1 Quality assurance officer will do extensive sampling of the process stage
6 wise as mentioned in the validation protocol.
4.3.2.1 These samples are transferred to quality assurance department for
7 analysis along with test request form and validation protocol.
4.3.2.1 After completion of testing, quality control will record the results of each
8 process in the data recording sheets provided in the validation protocol.
4.3.2.1 After getting compliance report from quality control, Production
9 department should start next process stage.
4.3.2.2 In process validation Sampling shall be done as per the sampling plan
0 illustrated in the diagram during each in process steps.
4.3.2.2 Test shall be performed at each stage during the process and results shall
1 be compared with the acceptance criterion.
4.3.2.2 Replicate studies must be conducted on minimum of three consecutive
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 CELEBRITY BIOPHARMA LIMITED
Format No.: QAS001/F/01/00 Reference SOP No.: SOP/QA/001/00
STANDARD OPERATING PROCEDURE
Location Quality Assurance SOP Number SOP/QA/038/00
Version 00
Superseded SOP No. Nil
Title Process Validation Effective Date
Review Date
Page Number 6 of 9

2 batches.
4.3.2.2 Note:
3
4.3.2.23.1 In the case of manufacturing process validation where
batch is manufactured on common blend concept, the
lowest strength will be considered for process validation.
4.3.2.23.2 The Challenging (i.e. subjected to sampling at different
time limits) of the critical Parameters (e.g. Mixing time,
RPM, Lubrication Time, and Hardness Challenges at
compression stages) will be done only on optimization
batches (Prospective Validation)
4.3.2.23.3 During concurrent validation the sampling shall be done at
fixed time interval as mentioned in Batch documents.
4.3.2.23.4 In case if BMR is having provision of multiple equipments,
ensure that each equipment is validated by taking three
consecutive batches.
4.3.2.23.5 For Example: If in BMR of XYZ 10mg, both 35 and 27
station compression machines included. Validate the 35
station compression machine on first three batches(A, B, C)
and 27 station compression machines on next three batches
(D, E, F).
4.3.2.23.6 In case validation of batches cannot be completed as per
approved protocol due to less marketing requirement or is
discontinued due to other justifiable reason then an
‘Interim Report’ shall be generated to give the status of
various parameters tested during validation studies.
However, process validation studies shall be deemed to be
completed only on successful completion of three batches.
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 CELEBRITY BIOPHARMA LIMITED
Format No.: QAS001/F/01/00 Reference SOP No.: SOP/QA/001/00
STANDARD OPERATING PROCEDURE
Location Quality Assurance SOP Number SOP/QA/038/00
Version 00
Superseded SOP No. Nil
Title Process Validation Effective Date
Review Date
Page Number 7 of 9

4.3.2.2 In cases where it is unlikely that second and / or Third batch of the
4 product will be manufactured for a period of time, generate interim
reports on batch to batch basis till such time the process validation study
is completed.
4.3.2.2 Deviations to Validation Protocol:
5
4.3.2.25. Any deviation from the approved protocol must be
1 documented and authorized.
4.3.2.25. In the event of acceptance criteria not being met, an
2 investigation shall be carried out to identify the root cause
and to provide corrective actions. If the investigation results
in a change to a process parameter or operations the
replication sequence shall start again and shall be conducted
on three batches.
4.3.2.2 If results of three batches are within acceptance parameters, giving the
6 product of desired quality, the process stands valid.
4.3.2.2 After completion of three validation batches, a conclusion will be written
7 with summary of results, duly certified by validation team for formal
acceptance.
4.3.2.2 Recommendation if any, necessary for routine production should be
8 incorporated in the Batch Manufacturing / Packing Record.
4.3.2.2 If any of the three batches do not meet acceptance criteria, revalidation
9 should be done.
4.3.2.3 Revalidation Criteria:
0
4.3.2.30. Change in primary packaging material and pack size.
1
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 CELEBRITY BIOPHARMA LIMITED
Format No.: QAS001/F/01/00 Reference SOP No.: SOP/QA/001/00
STANDARD OPERATING PROCEDURE
Location Quality Assurance SOP Number SOP/QA/038/00
Version 00
Superseded SOP No. Nil
Title Process Validation Effective Date
Review Date
Page Number 8 of 9

4.3.2.30. Change of any major equipment in the chain of equipments

2 which may affect the earlier validation study.
4.3.2.30. Any major modification to the equipment, which may affect
3 the earlier validation status.
4.3.2.30. If Batch Size is changed by ±10% of the Standard Batch
4 Size.
4.3.2.30. Based on any request from customer or regulatory agency.
5
4.3.2.3 Stability study of validation batches:
1
4.3.2.31. The validated batches shall be charged for stability as per
1 ICH Guideline.

5. RELATED DOCUMENTS
5.1 SOP No.: SOP/QA/042/00 : Master Document Numbering System
6. REFERENCES
6.1 Nil
7. RECORDS
7.1 Nil
8. ABBREVIATIONS
8.1 SOP : Standard Operating Procedure
8.2 QA : Quality Assurance
8.3 QC : Quality Control

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 CELEBRITY BIOPHARMA LIMITED
Format No.: QAS001/F/01/00 Reference SOP No.: SOP/QA/001/00
STANDARD OPERATING PROCEDURE
Location Quality Assurance SOP Number SOP/QA/038/00
Version 00
Superseded SOP No. Nil
Title Process Validation Effective Date
Review Date
Page Number 9 of 9

8.4 GMP : Good Manufacturing Practice.

8.5 ICH : International Conference On Harmonization
8.6 BMR : Batch Manufacturing Record
8.7 PVP : Process Validation Protocol
8.8 PVR : Process Validation Report
8.9 BPR : Batch Packaging Record
8.10 RPM : Rotation per Minute
9. REVISION RECORD

Version Reason for Revision Effective Date

00 New SOP --------
END OF DOCUMENT

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