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Stability Study Protocol

Table of Contents
  1. Objective
  2. Scope
  3. Responsibility
  4. Selection of Batches for Stability
  5. Sampling
  6. Stability Conditions
  7. Charging & Withdrawal of Samples
  8. Product Details
  9. Stability Attributes & Specifications
  10. Acceptance Criteria
  11. Stability Testing Schedule
  12. Stability Commitments
  13. Documentation & Reporting
  14. Conclusion
  15. References
  16. Revision History
  17. Annexures

Objective
The objective of this protocol is to define the procedure for carrying out a Stability study for XXX.

The quality of drug products is likely to be influenced during storage. Various factors are involved, such as temperature, humidity, primary packing, etc., affecting drug product quality. Therefore, it is necessary to evaluate the influence of these factors on product quality, establish the shelf life or evaluate storage conditions of the Drug Product (for new products). The stability is also carried out to ascertain that the existing products are stable until the end of their shelf life when studied per defined schedule/interval & stability conditions.

Scope
The scope of this Protocol is applicable to XXX.

The stability studies will be carried out to ensure the stability of the product till the end of its shelf life.

Responsibility
The Validation Team, comprising a representative from each of the following Departments, shall be responsible for the overall compliance of this Protocol:

Quality Assurance:

  • Preparation, Review, Approval, and Compilation of the Operation qualification Protocol cum Report.
  • Sampling

Quality Control:

  • Charging & Withdrawal of Samples – QС Chemist
  • Monitoring Temperature & Humidity Conditions of Stability Chambers – QС Chemist
  • Analysis of Stability Samples – QC Chemist Documentation & Reporting – Head QC



Selection of Batches 
Samples required for stability studies are taken by IPQA supervisors on the packing line and sent to the QC department.

The sample quantity of any subjected batch contains samples for the following requirements:
  • Sample required for one complete analysis for each time point.
  • Total quantity for all time points
  • One additional pack for any unforeseen event like OOS.
  • Placebo sample for each time point analysis.

Sampling
  • The sampling required for Stability Studies is to be drawn by IPQA Chemist on Packing Line. The samples to be taken should be in market equivalent containers i.e. In case it will be packed in Alu-Alu blister in a printed carton.
  • The sample quantity will be calculated to 1 pack extra in addition to the packs required for a single analysis.
  • The samples will be drawn by IPQA Chemists & then handed over to the QC department.
  • This will be recorded.

Stability Condition 
The products manufactured in the formulation plant will be subjected to 3
conditions: 
  1. Long Term Stability Studies at 25 ± 2°C / 60 ± 5% RH.
  2. Accelerated Stability Studies at 40 ± 2°C / 75 ± 5% RH. 
  3. Zone IVb. Long Term Stability at 30 ± 2°C / 75 ± 5% RH.

Charging & Withdrawal of Samples
  • The samples will be charged after putting the sticker labels on each pack.
  • The samples will have to be charged in the Stability chambers within 5 days of completion of the Initial Analysis.
  • As per the Calendar, the samples are withdrawn within 5 days of the due date of analysis for Long Term Stability Studies and Long Term Stability Studies for Zone IVb and 3 days of the due date of analysis for Accelerated Stability Studies.
  • The analysis of the samples will have to be done within 15 days from the due date of analysis.
  • In case of any deviation, this will be documented with justification & with approval from QA.


Product Details
XXX contains Paracetamol 500mg Tablets BP. The Product is packed in 10 x 10 Blister Pack.



CONTENTS:

Each uncoated tablet contains:

SHELF LIFE:

24 months

 

DOSAGE FORM:

Tablet

MANUFACTURED AT:

Pharmasky Ltd.

TYPE OF STABILITY STUDIES

Accelerated Stability Studies

40 ± 2°C

75 ± 5 % RH.

6 months

Long-Term Stability Studies

25 ± 2°C

60 ± 5 % RH.

36 months

Zone IVb. Long Term Stability

30 ± 2°C

75 ± 5 % RH.

36 months


Stability Attributes & Specifications

Sr. No.

Tests

Specifications

1

Description

White to off-white, round, flat, uncoated tablet, plain on both sides.

2

Identification

 

In the Assay, the principal peak in the chromatogram obtained with the test solution has the same retention time as the principal peak in the chromatogram obtained with the reference solution

3

Disintegration

NMT 15 minutes

4

Dissolution

NLT 75 % in 45 min

5

Assay

Between 95% to 105%

6

Uniformity of dosage units

XXX

7

Related substances

XXX


Acceptance Criteria
  • The Product is considered to be stable if it passes all the criteria for the Specifications mentioned above or if there is no significant change.
  • Significant change means:
  1. 5% change in assay form initial value or failure to meet the acceptance criteria 90% to 110% of the labeled amount.
  2. Related substances fail to meet the acceptance criteria.
  3. Fails to meet microbial purity.
  • Failure to meet the acceptance criteria for other parameters like Description, DT, Dissolution, Assay, Chromatographic Purity & Microbial Purity & any other characteristics.


Stability Testing Schedule
The stability Testing Schedule for XXX is as follows:

 

Accelerated

Long Term Stability

Zone IVb.

 

Tests

 

Initial

3

M

6

M

3

M

6

M

9

M

12

M

18

M

24

M

36

M

Description

 

 

 

 

 

 

 

 

 

 

Identification

 

 

 

 

 

 

 

 

 

 

Disintegration

 

 

 

 

 

 

 

 

 

 

Dissolution

 

 

 

 

 

 

 

 

 

 

Assay

 

 

 

 

 

 

 

 

 

 

Uniformity of dosage units

 

 

 

 

 

 

 

 

 

 

Related Substances

 

 

 

 

 

 

 

 

 

 

Microbial Purity

 

 

 

 

 

 

 

 

 

 


Stability Commitment
The product has been tested at the development stage (lab trial batches) for stability to determine the shelf life of the product. Besides, the first three commercial batches are kept for accelerated, long and Zone IVb. long-term stability. If required, accelerated stability study data shall be used for submission to authorities & Long term stability data will be provided as & when complete.

Documentation & Reporting
The analyst will enter the data obtained in the Stability Summary Report & at the end of completion of the Stability Study, a proper Report will be made with conclusions.

All the analytical Raw data carried out for stability will be retained in QC along with COA made for each sample from each station.

Conclusion
After completion of Long-Term Stability, Accelerated Stability Studies Stability, a conclusion about the assigned shelf life is to be drawn whether it can remain the same or it needs to be changed.

References
ICH Guidelines Q1A (R2)

Revision History
Nil

Annexures
All the entries of samples received for Stability analysis will be made in the documents as mentioned in the SOP for Stability Studies.

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