Performance Study
For a new product, formulation or container, and again after any change to the synthesis route, packaging or storage. Together with Comprehensive Release it completes the evidence for full APA designation.
Safety
Control what can cause harm.
01Mutagenic and nitrosamine riskAssessment and confirmatory testing for mutagenic and nitrosamine impurities.
The synthesis route, reagents and packaging are assessed for mutagenic and nitrosamine impurity risk. Where a risk is identified, confirmatory testing quantifies it against acceptable intake limits.
- Method
- Risk assessment with confirmatory LC-MS/MS
- Reference
- ICH M7, USP <1469>
Holistic peptide quality
Is it what the label says, at labeled strength?
02Functional potency and biological activityBiological activity relative to a reference standard.
The sample is tested in a cell-based assay for its target receptor and its potency reported relative to a reference standard.
- Method
- Cell-based receptor activation assay
03Binding affinityAffinity for the target receptor.Supporting assay; optional or bridging
Binding kinetics and affinity for the target are measured as a supporting assay, used on its own or to bridge between lots and formulations.
- Method
- Surface plasmon resonance
04Peptide mapping and full sequence confirmationComplete amino acid sequence and modifications.
The peptide is fragmented and the fragment ladder is read back against the expected sequence, confirming every residue and locating any modification.
- Method
- LC-MS/MS
05Stereochemical integrity and epimerizationD-amino acid content per residue.Select peptides
Racemization during synthesis produces D-amino acid variants with the same mass as the intended peptide. They are quantified per residue.
- Method
- Chiral amino acid analysis after hydrolysis
06Aggregation and self-association profileDimers, oligomers and higher molecular weight species.
Size-exclusion chromatography and light scattering report soluble aggregates and self-association that reverse-phase methods can miss.
- Method
- SEC-UPLC and dynamic light scattering
Manufacturing discipline and control
Does the vial stay in specification?
07Degradation pathways and forced degradationDegradation pathways under heat, light, oxidation and pH stress.
The product is stressed with heat, light, oxidation and pH. The result identifies the impurities to expect over time and demonstrates that the purity method can detect them.
- Method
- Stress conditions with UPLC-MS
- Reference
- ICH Q1A, Q1B
08Stability programPurity and content at controlled storage timepoints.
Purity and content are retested at set timepoints under long-term and accelerated storage, giving data behind the labelled shelf life.
- Method
- Timepoint testing at controlled conditions
- Reference
- ICH Q1A
09Container closure integrityDeterministic leak testing of sealed vials.
A deterministic leak test confirms that the vial, stopper and seal maintain sterility over the shelf life.
- Method
- Vacuum decay
- Reference
- USP <1207>
10Extractables and leachablesCompounds that migrate from the container into the product.
The container and closure are screened for extractable compounds and the product is tested for those that leach into it over time.
- Method
- LC-MS, GC-MS and ICP-MS screening
- Reference
- USP <1663> and <1664>
11Headspace gas and oxygen controlOxygen and gas composition in the sealed vial headspace.Oxidation-sensitive or inerted products
Headspace oxygen is measured non-destructively in sealed vials to confirm inerting for oxidation-sensitive products.
- Method
- Laser headspace analysis
Submit samples for Performance Study
The online submission generates an itemised invoice and a shipping packet.