The stability of a pharmaceutical product means how long it can keep its original form without any apparent changes affected by various environmental factors like temperature, humidity, light. In this SOP we will describe the Stability Testing of Pharmaceutical Products.
Page Contents
1. Purpose
It is established to ensure that the product maintains the specifications throughout the stated shelf life.
2. Scope
It is applicable in the Quality Assurance department to conduct Stability Testing of Pharmaceutical Products
ReferenceS
Product Test Method
ICH (Q1A2) (International Conference on Harmonization) and ICH Q1B
3.Responsibility
Manager Quality Assurance
Manager Quality Control
Assistant Manager Quality Control
Senior Quality Control Officer
4.Procedure
DESIGN OF STABILITY STUDY
Stability is the ability of the drug substance or drug product to retain its chemical, physical, microbial, and biological properties within specified limits throughout its shelf life under specified packaging and storage conditions.
Four climatic zones are distinguished for the purpose of worldwide stability testing. Pakistan is categorized in climatic zones 3 and 4
GENERAL STORAGE CONDITIONS (For Pakistan)
Accelerated Study: 40°C + 2°C / 75%RH + 5%RH
Long Term Study: 30°C + 2°C / 65%RH + 5%RH
SELECTION OF BATCHES
Stability information from accelerated and long term studies should be provided for three primary consecutive batches of the same formulation and dosage form in the containers and closure system proposed for marketing
TESTING FREQUENCY
Stability testing for long term studies generally should be performed at 3 months intervals during the first year, six months intervals during the second year, and yearly thereafter (e.g 0, 3, 6, 9, 12, 18, 24, 36 months)
For the accelerated storage conditions, a minimum of three test points including the initial and final time points
( e.g 0, 3, 6 months) is recommended
Where an expectation exists that results from accelerated storage are likely to approach significant change criteria, increased testing should be conducted either by testing additional samples at other time points in the protocol
(e.g 0, 1, 2, 3, and 6 months)
In general, the significant change for a product is defined as:
- A 5% change from its initial value; or failure to meet the acceptance criteria for potency.
- Any degradation product exceeding its acceptance criterion;
- Failure to meet the acceptance criteria for appearance, physical attributes, and functionality test (e.g. color, phase separation, resuspendability, caking, hardness); however, some changes in physical attributes (e. g. softening of suppositories, melting of creams) may be expected under accelerated conditions; and as appropriate for the dosage form;
- Failure to meet the acceptance criterion for pH; or
- Failure to meet the acceptance criterion for dissolution for 12 dosage units.
PROCEDURE:-
STABILITY STUDY (For New Products)
The Assistant Quality Control Manager receives the samples under development from the product development manager on the Interoffice memo and discusses with Manager Quality Control for inspection and testing.
Senior Officer Quality Control enters the details of the samples in Product Analysis Log (QAF-375) and does analysis at the time of receipt. Results are recorded in the raw data register and submitted to Manager Quality Control for recommendation
Manager Quality Control will discuss the results to Manager Quality Assurance for approval
Senior Officer Quality Control stores the samples in the ambient and accelerated conditions, do analyze (e.g 0, 3, 6 months) and results are recorded in the Product Stability Record Sheet (QAF-388)
A stability study of powder for suspension and injection also conducted to prove the label claim at ambient storage conditions.
STABILITY STUDIES (For Existing Products)
Senior Officer Quality Control keeps the samples at accelerated and ambient conditions, does analysis (e.g 0, 3, 6, 9, 12, 18, 24, 36 months), and maintains the raw data register QAF-375. After analysis, discuss the results with Manager Quality Assurance and get signed, records the result in Product Stability Record Sheet QAF-326.
In case of any change in the manufacturing process or formulation, again 3 consecutive batches will be kept for stability study at different conditions for the specific time period, after discussion with Manager Quality Assurance & Technical Director.
Note: Check Annual product review, For the determination of the stability of the product, a stability study and its trend are performed.
ICH Guidelines to Conduct Stability Testing
The extension and ideal behind ICH stability testing guidelines are to comprehend the shelf life of pharmaceutical drugs after being put away in various degrees of temperature, humidity, and light.
Batches: The selection of batches for a stability study should be the same as the ones that are chosen for distribution. The batches tested should be the same as the ones used in clinical trials and post packaging. The batches should be monitored for a period of 12 months and for those that were not approved for mass consumption in its first assessment should be observed for longer intervals.
Packaging: The packaging of products used for stability testing should be the same as the ones used during clinical trials and production.
Test Procedure: The test technique ought to require everything from efficiency, growth of microbial by-products, the formation of degradation products, the formation of crystalline by-products, the viscosity of the chemical, formation of moisture/water, and the effectiveness of the product.
Storage Conditions: The packaging material and the quality of the substance used while stability testing study should remain the same as the one submitted to the regulatory bodies in the clinical trials and production phase.
