Capsule: SOP for Shelf-Life Prediction Studies for Capsules – V 2.0

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Standard Operating Procedure for Shelf-Life Prediction Studies for Capsules

Department	Capsule Manufacturing
SOP No.	SOP/CM/046/2025
Supersedes	SOP/CM/046/2022
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 shelf-life prediction studies for capsules. These studies are critical in determining the stability and expiry date of capsules, ensuring their effectiveness, safety, and compliance with regulatory standards over time.

2. Scope

This SOP applies to the shelf-life prediction studies conducted for capsules during the development phase and during post-market surveillance. It includes the use of stability testing to assess the effect of environmental conditions (e.g., temperature, humidity, and light) on the capsules.

3. Responsibilities

Formulation Development Team: Responsible for designing the capsule formulation and ensuring it is suitable for stability testing based on the API, excipients, and packaging.
Manufacturing Team: Responsible for producing the capsules in accordance with the approved formulation, ensuring consistency in the production process for stability testing.
Quality Control (QC) Team: Responsible for conducting stability tests, such as dissolution, degradation, and physical characteristics, at various time intervals during the shelf-life study.
Quality Assurance (QA) Team: Ensures that the shelf-life prediction studies are performed in compliance with GMP and regulatory guidelines and that the data is accurately recorded and reported.

4. Accountability

The Capsule Manufacturing Supervisor is accountable for ensuring that the shelf-life prediction studies are executed as per this SOP. The QA Manager is responsible for reviewing the results and ensuring that the study adheres to regulatory requirements.

5. Procedure

5.1 Formulation Considerations for Shelf-Life Prediction

To conduct accurate shelf-life prediction studies, the following formulation considerations must be made:

Stability of Active Pharmaceutical Ingredient (API)
1. Assess the stability of the API in the final capsule formulation. API stability is influenced by factors such as pH, moisture, and temperature.
2. Select an appropriate dosage form, such as a matrix or capsule, that provides optimal protection against environmental factors that may degrade the API.
Excipients Selection
1. Ensure the excipients used in the formulation are stable and compatible with the API. Consider the impact of excipient degradation on the overall stability of the capsule formulation.
Packaging Considerations
1. Select suitable packaging materials (e.g., blister packs, bottles) that protect the capsules from light, moisture, and air, which can affect their stability.

5.2 Stability Testing Conditions

The following conditions should be established for stability testing during shelf-life prediction:

Storage Conditions
1. Store the capsules under controlled conditions, such as at elevated temperature (e.g., 40°C, 50°C) and humidity (e.g., 75% relative humidity), to accelerate degradation.
2. Include real-time storage at room temperature (e.g., 25°C, 60% relative humidity) as a control to simulate typical shelf-life conditions.
Light Exposure
1. If the formulation is light-sensitive, expose capsules to light to determine the effect of light exposure on stability. Use controlled light conditions such as UV light or incandescent light exposure for testing.
Packaging Variations
1. Conduct stability studies with different packaging formats to assess how packaging impacts the stability of the capsules over time.

5.3 Stability Testing Procedures

The following tests should be performed during the shelf-life prediction study:

Dissolution Testing
1. Conduct dissolution tests at multiple time points to assess the rate of drug release from the capsule under the stress conditions defined in the study.
2. Compare the dissolution profiles at different time intervals to detect any significant changes in release characteristics.
API Degradation Testing
1. Test for the degradation of the API over time, including quantification of degradation products, which could indicate a loss of drug potency or a potential increase in harmful impurities.
2. Conduct HPLC (High-Performance Liquid Chromatography) or other analytical methods to monitor API degradation and ensure that levels remain within acceptable limits.
Physical Characteristics Testing
1. Assess the physical properties of the capsules, including hardness, color, and appearance, to ensure that they remain consistent throughout the stability study.
Moisture Content Testing
1. Test the moisture content of the capsules periodically to ensure that the capsules are not exposed to excessive moisture that could affect the formulation’s stability.

5.4 Accelerated Stability Testing

In addition to real-time testing, accelerated stability studies can help predict the shelf life of capsules under stress conditions:

Temperature and Humidity Stress
1. Expose the capsules to elevated temperature (e.g., 40°C, 50°C) and relative humidity (e.g., 75%) to accelerate degradation and assess the impact on stability.
Testing Time Points
1. Perform tests at regular intervals (e.g., 3 months, 6 months, 12 months) and analyze the results to predict the shelf life based on accelerated degradation patterns.

5.5 Data Analysis and Shelf-Life Prediction

After conducting stability testing, analyze the data as follows:

Data Review
1. Review the results of dissolution, API degradation, physical characteristics, and other tests at each time point to determine any significant changes or trends.
Shelf-Life Estimation
1. Use the results from the accelerated stability testing to predict the shelf life of the capsules. This can be done by applying the Arrhenius equation or other predictive models to estimate the product’s shelf life at room temperature.

5.6 Documentation and Record-Keeping

Document all aspects of the shelf-life prediction studies:

Stability Study Protocol
1. Document the study protocol, including the objectives, storage conditions, testing procedures, and time points.
Testing Records
1. Maintain detailed records of all stability tests, including dissolution, degradation, and physical characteristics testing results, along with analytical data.
Final Shelf-Life Report
1. Prepare a final report summarizing the shelf-life prediction study, including all test results, data analysis, and the predicted shelf life of the capsules.

6. Abbreviations

SOP: Standard Operating Procedure
QA: Quality Assurance
QC: Quality Control
API: Active Pharmaceutical Ingredient
GMP: Good Manufacturing Practice
HPLC: High-Performance Liquid Chromatography

7. Documents

Stability Study Protocol (Annexure-1)
Stability Testing Records (Annexure-2)
Final Shelf-Life Report (Annexure-3)

8. References

USP <711> – Dissolution Testing
FDA Guidance for Industry: Stability Testing of Drug Products
International Conference on Harmonization (ICH) Guidelines for Pharmaceutical Development

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

Protocol ID	Description	Approval Status
SSP-001	Stability Study for Capsule Formulation	Approved

Annexure-2: Stability Testing Records

Batch ID	Storage Condition	Test Type	Result
Batch 001	40°C, 75% RH	Dissolution	Pass

Annexure-3: Final Shelf-Life Report

Batch ID	Predicted Shelf Life	Comments
Batch 001	24 months	No significant degradation

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 testing protocol	Standardization	QA Head