Capsule: SOP for Stability Studies During Formulation Development – V 2.0

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Standard Operating Procedure for Stability Studies During Formulation Development

Department	Capsule Manufacturing
SOP No.	SOP/CM/038/2025
Supersedes	SOP/CM/038/2022
Page No.	Page 1 of 7
Issue Date	01/02/2025
Effective Date	05/02/2025
Review Date	01/02/2026

1. Purpose

The purpose of this SOP is to define the procedure for conducting stability studies during capsule formulation development. Stability testing ensures that the developed formulation maintains its intended quality, safety, and efficacy over time under various environmental conditions.

2. Scope

This SOP applies to all new capsule formulations being developed. Stability studies are critical in the early stages of formulation development to identify potential degradation, optimize shelf life, and determine appropriate storage conditions.

3. Responsibilities

Formulation Development Team: Responsible for selecting the formulation, determining the stability testing parameters, and performing initial stability evaluations.
Quality Control (QC) Team: Responsible for conducting the stability testing, including storage conditions, testing frequency, and data analysis of the samples.
Quality Assurance (QA) Team: Ensures the stability study is conducted following regulatory requirements and company standards and reviews all records and reports for compliance.
Regulatory Affairs Team: Ensures that the stability study protocols and results comply with the regulatory requirements for market authorization.

4. Accountability

The Capsule Manufacturing Supervisor is accountable for ensuring that stability studies are conducted as per this SOP and that all relevant data is accurately recorded. The QC Manager is responsible for overseeing stability testing, while the QA Manager ensures compliance with regulatory guidelines.

5. Procedure

5.1 Stability Study Planning

Before initiating stability studies, the following steps should be taken:

Define Study Objectives
1. Determine the purpose of the stability study, including the intended shelf life of the formulation and the conditions it must endure.
2. Establish the critical quality attributes (CQAs) of the formulation that will be monitored during stability testing (e.g., API potency, dissolution, appearance, moisture content).
Set Storage Conditions
1. Select the storage conditions under which the stability study will be conducted. Conditions typically include controlled room temperature (CRT), accelerated stability conditions (e.g., 40°C/75% RH), and long-term storage conditions (e.g., 25°C/60% RH).
Determine Testing Intervals
1. Define the frequency of testing, which may include time points such as 0, 1, 3, 6, 9, and 12 months, depending on the study requirements and regulatory guidelines.
Establish Control Samples
1. Prepare control samples under the same conditions for comparison purposes during the stability testing period.

5.2 Stability Study Execution

Conduct stability studies according to the plan outlined above:

Sample Preparation
1. Prepare the required quantity of capsule dosage forms for stability testing, ensuring that they are representative of the final batch.
Storage Under Defined Conditions
1. Store the samples under the selected conditions, ensuring that they are maintained in the designated stability chamber or storage area.
Monitoring of Storage Conditions
1. Regularly monitor and document the temperature and humidity levels within the storage area to ensure that the environmental conditions are within the specified ranges.
Periodic Testing
1. At the predetermined time points, remove the samples from storage and perform the necessary testing as per the defined protocol.
2. Tests should include evaluations of the appearance, dissolution, content uniformity, assay, moisture content, and any other parameters relevant to the formulation’s stability.

5.3 Data Analysis and Reporting

Analyze the stability test results and prepare the stability report:

Data Collection
1. Collect and organize all testing data, ensuring that the results are recorded in a consistent and accurate manner.
2. Track any deviations from the expected results, and document the reasons for such deviations, if applicable.
Statistical Analysis
1. Perform statistical analysis, if necessary, to determine whether the capsule formulation meets the defined specifications over time.
2. Review the trend of key quality attributes, such as potency or dissolution, and determine if they remain within the acceptable range.
Stability Report
1. Prepare a comprehensive stability report summarizing the test results, observations, and conclusions. The report should include the following:

5.4 Adjustments Based on Stability Results

If the stability study reveals any issues with the formulation’s performance, make necessary adjustments:

Reformulation
1. If the formulation shows signs of instability (e.g., degradation of the API, changes in dissolution), consider modifying the formulation by adjusting excipients or adding stabilizers.
Packaging Changes
1. If packaging is identified as a contributing factor to instability, explore alternatives such as moisture-proof packaging or blister packs.
Storage Condition Adjustment
1. If stability problems arise under the current storage conditions, reassess and adjust the recommended storage temperature and humidity range.

5.5 Documentation and Record-Keeping

Maintain accurate and up-to-date records of all stability study activities:

Stability Testing Records
1. Document all data and test results in a clear, organized manner, ensuring they are easy to access for review and regulatory compliance purposes.
Stability Study Report
1. Ensure that the final stability study report is signed off by the responsible personnel, including the QA Manager, to confirm that the formulation meets stability requirements.
Archiving
1. Store all stability testing records and reports in accordance with company policies and regulatory guidelines for future reference and audits.

6. Abbreviations

SOP: Standard Operating Procedure
QA: Quality Assurance
QC: Quality Control
API: Active Pharmaceutical Ingredient
GMP: Good Manufacturing Practice
RH: Relative Humidity
USP: United States Pharmacopeia

7. Documents

Stability Study Protocol (Annexure-1)
Stability Test Report Template (Annexure-2)

8. References

USP <1191> – Stability Testing of New Drug Substances and Drug Products
FDA Guidance for Industry: Stability Testing of Drug Products
International Conference on Harmonization (ICH) Q1A – Stability Testing of New Drug Substances and Products

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Stability Study Protocol

Study ID	Storage Condition	Test Points	Duration
Study A	25°C / 60% RH	0, 3, 6, 12 months	12 months

Annexure-2: Stability Test Report Template

Test Type	Test Result	Specification	Remarks
Dissolution	Pass	Within USP Limits	No deviation

Revision History:

Revision Date	Revision No.	Revision Details	Reason for Revision	Approved By
01/01/2024	1.0	Initial Version	New SOP Creation	QA Head
01/02/2025	2.0	Updated stability study methodology	Standardization	QA Head