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Q5C Quality of Biotechnological Products: Stability Testing of Biotechnological/Biological Products

FinalCenter for Drug Evaluation and Research Center for Biologics Evaluation and Research07/01/1996
Stability TestingProcess ValidationStability-Indicating Profile

Description

The guidance stated in the ICH harmonized tripartite guideline entitled “Stability Testing of New Drug Substances and Products” (issued by ICH on October 27, 1993) applies in general to biotechnological/biological products. However, biotechnological/biological products have distinguishing characteristics to which consideration should be given in any well-defined testing program designed to confirm their stability during the intended storage period. For such products in which the active components are typically proteins and/or polypeptides, maintenance of molecular conformation and, hence, of biological activity, is dependent on noncovalent as well as covalent forces. The products are particularly sensitive to environmental factors such as temperature changes, oxidation, light, ionic content, and shear. To ensure maintenance of biological activity and to avoid degradation, stringent conditions for their storage are usually necessary.

Key Topics

Terms and concepts identified from this document

Scope & Applicability

Product Classes

7
Biotechnological Products

Example of a control strategy summary for biological drug substances

Biological Products

Requires analytical comparability per ICH Q5E

Biotechnological/Biological Products

Covered by GFI #99

Vaccines

Products for which batch/lot information is particularly important

Monoclonal Antibodies

Circumstance where a mass balance study might not be recommended

Biotechnological/Biological Product

General category of products covered by the stability testing guidance.

Drug Product

RTRT and CTD sections apply to drug products

Stakeholders

1
Applicant

Entity submitting development data and knowledge; Entity performing the work process for change

Regulatory Context

Regulatory Activities

1
Marketing applications

Submissions where clinical trial reports must meet ICH E3 standards.

Document Types

3
Protocol

Defines the standard of veterinary practice and limits for anesthetic regimens

Dossier

approved design space described in the dossier

Stability Protocol

Protocol design for formal stability studies; Incorporates information to establish re-test period or shelf life; Design and execution of a stability protocol to support formal studies; Design for supporting drug substance or drug product shelf life; Design of the stability study including frequency and conditions; Written protocol for holding time studies; Design of in-use stability study protocols; Reduced Stability Protocol Design discussed in Annex 1; Including intermediate storage condition

Attributes

6
Potency

Measurement of potency for biological products

Storage temperatures

Precisely defined storage temperatures are recommended

Purity

specifications for the purity, strength, and composition of dietary supplements

Expiration dating

Specified in the product label based on stability studies

Shelf Life

Determined based on stability data; Established through stability testing; also called dating period.; Established through formal stability studies; Establishing the period during which a drug product is expected to remain within specifications; Period for drug products; The period during which a drug product is expected to remain within specifications; Duration product remains within acceptance criteria; Period during which product remains within specifications; Established for intermediates pu

Expiration Dating Period

CMC changes after tentative approval; shelf-life period supported by stability data; proposing to extend the expiration dating period for the drug product

Technical Details

Substances

9
Proteins

Products composed of well-characterized proteins

Intermediate

A material produced during steps of the synthesis that undergoes further molecular change.

Impurity

Any component of the drug substance or drug product which is not the active ingredient or excipient

Degradation Product

Molecular variants or impurities resulting from chemical or biochemical changes; Shelf Life Estimation Based on a Degradation Product

Conjugated Product

Active ingredient bound covalently or noncovalently to a carrier

Polypeptides

Products composed of well-characterized polypeptides

Recombinant deoxyribonucleic acid

r-DNA technology used for production

Drug Substance

Postapproval changes to drug substances; the active pharmaceutical ingredient being modified; Evaluation of physical properties for drug substance; Active ingredient intended to furnish pharmacological activity; The molecule or ion responsible for the physiological or pharmacological action.; The active pharmaceutical ingredient subject to postapproval changes

Adjuvant

CQAs should be evaluated during vaccine stability studies

Testing Methods

9
Assays for biological activity

Should be part of pivotal stability studies

Statistical methods

sponsors should propose statistical methods that properly account for missing data

Immunochemical methods

Methods for analysis of the molecular entity

Matrixing

study designs generally inappropriate for recombinant protein products

Bracketing

study designs generally inappropriate for recombinant protein products

Electrophoresis

Analytical method specified in LOINC 2862-7

High-Resolution Chromatography

Includes reversed-phase, gel filtration, and ion exchange chromatography.

Peptide Mapping

Complementary analytical technique

Sterility Testing

Product-specific sterile process validation question

Processes

7
Fermentation

Production method requiring additional information in a notification; Manufacturing process using microorganisms like bacteria or yeast.; Changing conditions to alter the chemical or molecular composition.; ingredients produced using fermentation; information about the organism and fermentation process; relevant to safety and identity of microorganisms; NDI produced by fermentation using microorganisms

Pilot-Plant Scale

Production by a procedure fully representative of manufacturing scale

Manufacturing Scale Production

Manufacture at the scale typically encountered in a facility for marketing

Real-time stability studies

Conducted monthly for the first 3 months

Purification

Preferable to rely on purification processes to remove impurities

Lyophilization

Physical modification that does not result in chemical alteration.; A process that does not typically chemically alter an ingredient

Reconstitution

Automated mixing of drug prior to injection.

Identified Hazards

Hazards

4
Oxidation

Environmental factor causing degradation; A chemical degradation change that may occur during storage.

Temperature changes

Environmental factor causing degradation

Deamidation

A chemical degradation change that may occur during storage.

Aggregation

Mechanism of product degradation

Standards & References

External Standards

1
International Reference Material

Standards used to calibrate potency assays across different laboratories.

Specifications

4
Process limits

Limits established for intermediates to assure stability

End of shelf life specifications

Distinct release and end of shelf life specifications

Release specifications

Criteria that must be met before product release

Acceptable Degradation Limits

Limits derived from analytical profiles of batches used in clinical studies.

ICH References (1)

ICH Q5C

Quality of Biotechnological Products: Stability Testing

Related MFDS Guidelines

Korean regulatory guidelines covering similar topics

See Also (8)