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Q1A(R2) Stability Testing of New Drug Substances and Products

FinalCenter for Drug Evaluation and Research Center for Biologics Evaluation and Research11/21/2003
Stability CommitmentValidation

Description

This guidance is the second revision of Q1A Stability Testing of New Drug Substances and Products, which was first published in September 1994 and revised in August 2001. The purpose of this revision is to harmonize the intermediate storage condition for zones I and II with the long-term condition for zones III and IV recommended in the ICH guidance Q1F Stability Data Package for Registration Applications in Climatic Zones III and IV. The changes made in this second revision are listed in the attachment to this guidance.

Key Topics

Terms and concepts identified from this document

Scope & Applicability

Product Classes

2
New Molecular Entities

Mass balance studies should be conducted for all new molecular entities

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

2
Registration Application

data which should be presented in a registration application

Stability Commitment

A commitment to continue stability studies post-approval

Document Types

2
Stability protocol

Post-approval stability protocol changes

Labeling

Cybersecurity information should be included in device labeling

Attributes

10
Mean Kinetic Temperature

Derived from climatic data to define testing conditions; Single derived temperature affording the same thermal challenge as a range of temperatures

Storage condition tolerances

Acceptable variations in temperature and relative humidity

Retest date

conclusions regarding appropriate storage conditions and an appropriate retest or expiration date; a retest date allows for use of a material beyond the retest date

Production batch

A batch manufactured at production scale using production equipment in a production facility.

Primary batch

A batch used in a formal stability study from which data are submitted in a registration application.

Pilot scale batch

A batch manufactured by a procedure fully representative of a full production scale batch.

Expiration date

should be based on appropriate supportive stability data

Water loss rate

Measured at specific relative humidity and temperature to assess semipermeable containers.

Storage Conditions

Long-term, accelerated, and intermediate conditions

retest period

proposed for a drug substance; Proposing a retest period or shelf life based on attribute assessment; period established for drug substances based on stability data

Technical Details

Substances

3
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

New molecular entity

Drug type that may alter the minimum acceptable size of the safety database

Excipient

Component used in human and animal drugs

Testing Methods

9
Photostability testing

Used to suggest potential for photoreactivity

Stress testing

Product testing after storage under exaggerated conditions

Mass balance

The process of adding together the assay value and levels of degradation products.

Long-term testing

Stability studies under the recommended storage condition for the retest period or shelf life.

Intermediate testing

Studies conducted at 30°C/65% RH designed to moderately increase the rate of chemical degradation.

Statistical analysis

Used to demonstrate that results of testing are poolable for grouped sensors

linear regression analysis

used to represent the relationship between an attribute and time

Bracketing

study designs generally inappropriate for recombinant protein products

Matrixing

study designs generally inappropriate for recombinant protein products

Processes

10
Bracketing

Alternative approach to stability protocol design; A reduced stability design testing only extremes of certain factors.; An example of a bracketing design is given in Table A1-1; If a bracketing design is utilised

Formal stability studies

Long-term and accelerated studies undertaken on primary and/or commitment batches.

Stability Testing

Primary process described in the guideline; Core activity described in the guidance; General process for evaluating product quality over time; Formal stability studies to assess adjuvant stability; Evaluation of attributes at all storage conditions; The process of evaluating product quality over time under specified conditions.; Evaluation of product quality over time

Stress Testing

Testing to identify degradation products and pathways; Studies undertaken to elucidate intrinsic stability of drug substances or medicinal products

Photostability Testing

Purpose of photostability testing for drug substances.; Evaluation of light exposure effects on product efficacy; Systematic approach to testing light-sensitive products; Required if product is sensitive to light exposure; Testing for light sensitivity in reduced protocol designs

Accelerated storage condition

40°C ± 2°C / 75% RH ± 5% RH

Long-term storage condition

25°C ± 2°C/60% RH or 30°C ± 2°C/65% RH

Intermediate storage condition

30°C ± 2°C / 65% RH ± 5% RH

Stability Studies

Testing conducted to ensure expiration dating and storage conditions

Accelerated testing

Studies designed to increase the rate of chemical degradation or physical change using exaggerated storage conditions.

Standards & References

Specifications

8
Shelf Life

Confirmed by 3 months of stability data

Shelf life Specification

Tests and acceptance criteria determining suitability throughout retest period or shelf life.

Release Specification

Combination of tests and acceptance criteria determining suitability at the time of release.

Acceptance criterion

Specific limits used to define specified or unspecified impurities.

Retest Period

establish a retest period for the drug substance

acceptance criteria

Criteria for security architecture and design outputs.

Shelf life acceptance criteria

Criteria to ensure quality through the end of shelf life

Significant change

Defined as 5 percent change in assay or failure to meet physical attributes

ICH References (9)

ICH Q1A(R2)

Stability Testing of New Drug Substances and Products

ICH Q1F

Stability Data Package for Registration Applications in Climatic Zones III and IV.

ICH Q5C

Quality of Biotechnological Products: Stability Testing

ICH Q1C

Stability Testing for New Dosage Forms

ICH Q1B

Photostability Testing of New Drug Substances and Products

ICH Q6A

Referenced regarding specifications and solid state forms.

ICH Q6B

Specifications for biotechnological/biological products; Specifications: Test Procedures and Acceptance Criteria for Biotechnological/Biological Products

ICH Q3A

impurities in new drug substances; Referenced regarding impurities and polymorphism.

ICH Q3B

impurities in new drug products; Impurities in new drug products; Recommendations for genotoxicity studies and toxicological qualification; Impurities in New Drug Products; Qualification study(ies) as described in ICH Q3B

Related MFDS Guidelines

Korean regulatory guidelines covering similar topics

See Also (8)

Q1A(R2) Stability Testing of New Drug Substances and Products | Guideline Explorer | BioRegHub