You want to carry out an analysis of chemical contamination in lyophilisates
What is a lyophilisate?
A lyophilisate is a solid, dry product created by lyophilisation, or drying by sublimation. This unique process involves freezing a liquid product (solution, suspension, extract, etc.) and removing the water in vapour form, without ever allowing it to return to the liquid state.
The result is a light, porous and very dry substance, which retains its original chemical, biological or pharmaceutical properties. Lyophilisates are mainly used to improve the stability, shelf life and ease of transport of moisture- or heat-sensitive products.
Why carry out an analysis of chemical contamination in lyophilisates?
Lyophilisates, used in particular in the pharmaceutical, biotechnology and cosmetics sectors, are highly purified and stable forms of product. However, the manufacturing process and the materials used can introduce chemical impurities which, even at very low levels, can have significant consequences.
Consumer safety
Efficiency and product integrity :
Strict regulatory compliance :
Identifying the source of problems
Process optimisation and validation
Types of contaminants frequently sought
Solvants résiduels : issus des étapes de synthèse ou de purification.
Métaux lourds : provenant des réactifs, des catalyseurs ou des équipements.
Impuretés liées au processus : sous-produits, réactifs non transformés.
Composés extractibles et relargables : libérés par les contenants ou les matériaux de conditionnement.
Produits de dégradation : résultant de l'instabilité du produit lui-même ou des interactions avec l'environnement.
Résidus de nettoyage : détergents ou désinfectants.
Silicone : issu des joints, des tuyaux ou des lubrifiants d'équipement, notamment dans l'industrie pharmaceutique et des dispositifs médicaux.
Quality Risk Management (QRM) and analysis of lyophilisate contamination
Quality Risk Management (QRM) is a systematic and preventative method essential for the pharmaceutical and biotechnology sectors. Its objective is to identify, assess, control, communicate, and review risks affecting product quality.
Applied specifically to the analysis of lyophilizate contamination, QRM allows for the development of a robust and relevant analysis strategy. It involves identifying potential sources of contamination (raw materials, personnel, equipment, environment, packaging), estimating the probability and severity of these contaminations, and then implementing appropriate control measures.
This risk-based approach ensures that analysis efforts are focused on the most critical points. This optimizes product safety, regulatory compliance, and the effectiveness of quality controls, while avoiding unnecessary analysis.
The FILAB laboratory can help you analyse chemical contamination in lyophilisates
Why choose FILAB for the analysis of chemical contamination in lyophilisates?
When you choose FILAB to analyse the chemical contamination of your freeze-dried products, you are choosing a laboratory with expertise in physico-chemical analysis, capable of characterising your products in detail: residual moisture, structure, purity, stability, contaminants.
Our state-of-the-art analytical facilities enable us to respond to all kinds of problems, from development to batch release.
We provide tailor-made support, with an analysis plan adapted to your technical, regulatory or customer constraints.
Our resources
Organic chemical analysis
GC/MS, Py-GCMS, UPLC-MSMS, LC-QTOF-MS, LC-QTOF-MS, LC-ORBITRAP, GPC, NMR, FTIR
Powder analysis
XRD, SEM-FEG EDX, BET, Laser Granulometry
Mineral chemical analysis
ICP, XRD, IC
Thermal analysis
TGA, TGA-FTIR, DSC
Surface characterization
SEM-FEG EDX, XPS, TOF-SIMS
FAQ
Chemical contamination in a lyophilisate refers to the presence of any undesirable substance that is not supposed to be there. These impurities can come from raw materials, the manufacturing process, equipment, packaging materials or even the environment. They can include residual solvents, heavy metals, plasticisers, degradation products, cleaning residues or silicones, among others.
Analyses can be carried out at several stages to improve risk control:
- Control of raw materials: to ensure that the initial components are free from contaminants.
- In-process control (IPC): to rapidly detect any contamination introduced during the process.
- Finished product analysis: the final validation before the batch is released onto the market.
- Stability studies: to monitor the appearance of contaminants or degradation products over time.
- Non-conformity investigations: when unexpected quality problems arise.
Packaging materials can be a major source of contamination by leaching (release of chemical substances from the material into the product) or extraction (migration of substances into the product under certain conditions). Plasticisers, residual monomers, glidants and surface treatment residues (such as the silicone often used to lubricate syringes or vials) can migrate into the lyophilisate. Specific leaching/extraction studies are therefore essential.
Requirements vary according to product type and geographical region, but are generally very strict:
- Specification limits: defined by pharmacopoeias (USP, Ph. Eur., JP) or by specific guidelines for impurities.
- Impurity qualification: impurities above a certain threshold must be identified, characterised and their toxicological impact assessed.
- Method validation: the analytical methods used must be validated according to strict criteria (specificity, linearity, accuracy, precision, limit of detection, limit of quantification).
