CEI-MS-13 — Development and validation of a stability-indicating method for peptide preparations
Development and validation of a stability-indicating method for peptide preparations
§1Scope
§1.1Scope
Applies to the validation of any chromatographic method intended to support a purity or content claim over time. A method that has not been shown to separate the analyte from its degradation products cannot detect degradation and cannot support a shelf-life or in-use claim.
§2Principle
A method is stability-indicating when it resolves the analyte from every degradation product generated under forced-degradation conditions, with demonstrated peak purity and mass balance. Forced degradation deliberately generates the degradants that real storage will produce more slowly, so that the method can be shown to see them before it is relied upon.[1,2]
§3Apparatus and reagents
§3.1Apparatus
- HPLC or UHPLC with diode-array detection for peak-purity assessment
- LC–MS for degradant identification
- Photostability chamber meeting the ICH option 2 requirements
- Thermostatted ovens and controlled-humidity chambers
- pH meter and analytical balance
§3.2Reagents and reference materials
- Hydrogen peroxide 0.3–3 % for oxidative stress
- Hydrochloric acid and sodium hydroxide, 0.1 M, for hydrolytic stress
- Buffers spanning pH 2 to 10
- Reference standard and a control sample stored at −20 °C
References cited on this page
References are numbered in order of first citation in this document. Each superscript in the text links to its entry below.
- International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use. ICH Q2(R2) Validation of Analytical Procedures. ICH Harmonised Guideline 2023;Step 4 version, 1 November 2023. identifier not held by the Institute
- International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use. ICH Q1A(R2) Stability Testing of New Drug Substances and Products. ICH Harmonised Tripartite Guideline 2003;Step 4 version. identifier not held by the Institute
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