SOP for Stability Study

 

 

1.0           Purpose

1.1      To describe the procedure for collection, storage, analysis of stability samples and stability report preparation of finished products of lab batches, validation batches and on-going stability batches for HRM products and to provide guidance on how stability studies perform under different environmental conditions such as temperature, light and humidity and shelf life declaration on the basis of stability study data.

2.0           Scope

2.1         This SOP is to be followed to prepare stability study protocol, collection of stability samples their storage, withdrawal, analysis and reporting in Product Development & Quality Control Department of "NAME" Pharmaceuticals Ltd.

3.0           Responsibility

3.1.          Stability study protocol and report for lab batch and validation batch will be prepared & checked by Product Development, Officer/Asst. Manger and approved by Head of Quality Assurance (both of validation batch & lab batch)

3.2.          In-case of lab batches--

3.2.1        After completion of successful lab trial, Product Development shall be responsible to pack the product with desired packaging mode. Then make the proper labeling & store according to protocol.

3.2.2        Product Development (Support Quality Control) shall be responsible to analyze the stability samples time to time according to protocol and prepare summary report.

3.3.          In-case of validation batches--

3.3.1        Concerned QA Officer shall be responsible to collect samples from validation batches according to process validation protocol and send to concern Officer/ Sr. Officer of Product Development.

3.3.2        Product Development shall be responsible to receive the samples and labeling & store according to stability protocol.

3.4.          In-case of commercial batches--

3.4.1      Concerned QA Officer shall be responsible to collect samples from on-going stability study batch according to process validation protocol and send to concern Officer/ Sr. Officer of Quality Control development.

3.4.2      Quality Control shall be responsible for receive the samples and labeling & store the sample in stability chamber according to stability study protocol.

3.5.          Head of QA and Head of Product Development are accountable for this SOP.

4.0           Abbreviations and Definitions

4.1            SOP= Standard Operating Procedure

4.2            QA= Quality Assurance

4.3            PD= Product Development

4.4            QC= Quality Control

4.5            DRA= Drug Regulated Affairs

4.6            HRM= High Regulatory Market

4.7            ICH= International Conference on Harmonization

4.8            TGA= Therapeutic Goods Administration

4.9            GMP= Good Manufacturing Practices

4.10          RH= Relative Humidity

4.11          UV=Ultra Violet

4.12          ACI= Anderson Cascade Impactor

4.13          MI= Manufacturing Instruction

4.14          Stability Study: Stability study is evidence on how the quality of a drug product varies with time under influence of a variety of environmental factors such as temperature, humidity and light and enables recommended storage conditions, reset periods and shelf-lives to be established.

5.0           Materials and Equipment

5.1            Not Appreciable

6.0           Precaution / Health and Safety Considerations

6.1            Stability study protocol must be prepared and approved before keeping sample in the stability chamber for stability study of a product.

6.2            All information should be clearly written in protocol.

6.3        Labeling on the product and storages & withdrawal log book must maintain carefully to avoid further difficulties.

6.4            Stability samples (for validation batch) to be stored within 10 days of finished product releasing.

7.0           Procedure

7.1            Stability study protocol-

7.1.1    Stability study protocol will be described the procedure to perform the stability program for every individual product formulation.

7.1.2    The protocol will be applicable for PD lab batches, validation batches & on-going stability study batches.

7.1.3    The protocol will contain product related information and a protocol No. to identity the protocol individually and the date of preparation should be mentioned.

7.1.4    Product formulation will be mentioned in the protocol for lab batches, product formulation of validation batch and on-going stability study is available in the batch document.

7.1.5    Following information will be mentioned in the protocol.

7.1.5.1        Protocol No.

7.1.5.2        Product name

7.1.5.3        Generic name & strength

7.1.5.4        Dosage form

7.1.5.5        Label claim

7.1.5.6        Batch No.

7.1.5.7        Batch size

7.1.5.8        MI No. (In-case of validation and on-going stability batch)

7.1.5.9        Sample Quantity

7.1.5.10      Manufacture of active drug substance

7.1.5.11      Mfg. Date

7.1.5.12      Exp. Date (in-case of validation and on-going stability batch)

7.1.5.13      Manufacturing site (in-case of validation and on-going stability batch) 

7.1.5.14      Reason for study

7.1.5.15      Product formulation (in-case of lab batch)

7.1.5.16      Details of packaging component

7.1.5.17      Test parameter to be performed

7.1.5.18      Specifications

7.1.5.19      Test schedule, storage conditions

7.1.5.20      Name of persons prepare, checked & approved the protocol.

7.2            Execution of stability

7.2.1      After proper labeling, the received samples (in-case of validation & on-going stability batch) and successful trial samples (in-case of lab batch) to be stored, where Product name, batch No., Storage condition and Storage date will be mentioned.

7.2.2      Fill the storage & withdrawal log book for real time condition of validation batches, for accelerated condition of lab & validation batches, for real time condition of lab batches and on-going stability study batches. Different log books will be issued for different conditions.

7.2.3        Store the different quantity samples in different conditions stability chambers as per stability study protocol.

7.2.4        During withdrawal of stability sample fill storage & withdrawal log book and maintain inventory.

7.2.5        Analyze the stability sample as per stability protocol.

7.2.6        Stability study protocol numbering system is Dept. SP-XXX/YY. Where Dept.= Department name (i.e. PD or QC), SP= Stability Protocol, XXX= Sequential number & YY== Last two digit of year.

7.2.7        Monthly stability schedule to be prepared and approved at the end of previous month.

7.2.8        In-case of lab batch-Stability study to be continued up to Six (06) months for all conditions. Testing frequency for lab batches will be initial, three (03) months and six (06) months.

In-case of lab batch for refrigerated products, stability study to be continued up to twelve (12) months & testing frequency for lab batches will be initial, three (03) months, six (06) months, nine (09) months & twelve (12) months.

For special requirement, additional testing frequency can be added in stability study protocol.

In-case of validation batch, stability study to be continued up to six (06) months for accelerated condition & shelf life plus one year for real time condition. Testing frequency for validation batches will be initial, three (03) months interval in first year, six (06) months interval in second year, nine (09) months & twelve (12) months interval thereafter.

For special requirement, additional testing frequency can be added in stability study protocol.

In-case of on-going stability study batch, stability study to be continued on one batch per year (first batch of the year/first batch after completing process validation) of each product, each strength and each individual packaging and carried out for long term at real time condition (target market country) over the period of labeled shelf life with three (03) months interval in first year, six (06) months interval in second year, nine (09) months & twelve (12) months interval thereafter.

7.2.9        Photo stability study to be conducted for light sensitive products according to stability study protocol.

7.2.10      Stability samples can be withdrawn from the chamber on due date or maximum one week earlier up to 06 (six) months stability study and keep in ambient condition. In-case of refrigerated product sample will be withdrawn on due date.

7.2.11      Stability samples can be withdrawn from the chamber on due date or maximum two weeks earlier for more than 06 (six) months stability study and keep in ambient condition. In-case of refrigerated product sample will be withdrawn on due date.

7.2.12      Analysis of stability samples up to 06 months to be conducted within 1 week earlier or two weeks later on due date.

7.2.13      Analysis of stability samples more than 06 months to be conducted within 2 weeks earlier or 1 month later on due date.

7.2.14      After completion of stability analysis result to be calculated in stability test record sheet.

7.2.15      Microbial limit test to be conducted at initial and after six (06) months for lab batches, samples taking from real time condition for non-sterile products as per protocol.

7.2.16      Microbial test (limit test, particulate matter etc.) to be conducted at initial and the end of shelf life for validation and on-going stability study batches, samples taking from real time condition for non-sterile products as per protocol.

7.2.17      If the analytical and/or microbial results are out of specification, the result must be investigated and reported.

7.2.18      Summary of stability study result also to be prepared, checked and approved as per standard format.

7.2.19      Summary of stability study result also to be prepared, checked and approved as per standard format.

7.2.20      Stability study report numbering system is Dept. SR-XXX/YY. Where Dept.= Department name (i.e. PD or QC), SR= Stability Report, XXX= Sequential number & YY== Last two digit of year. Sequential number will be same as protocol.

7.2.21      Initial data of validation and on-going stability batch to be collected from finished product analytical report.

8.0           Reference Document

8.1            ICH guidelines Q1A (R2), Q1B

9.0           Annexure

9.1            Not Appreciable

10.0        Revision History

 

Revision No.	Brief reason for the revision	Effective Date	Remarks
01	New
02

11.0        Training

11.1        Head of Product Development or his/her nominee shall give the SOP training before effective date.