Analytical Testing Services

• QC testing for raw material and finished product release
• Reference standard qualification
• Full physical and chemical characterisation to support formulation development
• ICH stability testing
• Impurity testing (e.g., extractables and leachables, MCPD, and nitrosamines)

Method Development: Our experienced team develops robust analytical methods using a quality by design (QbD) approach as per ICHQ14 to support drug product development at different stages. Methods are evaluated for sensitivity, selectivity, linearity, accuracy, and precision as an essential part of method development. Design and execution of forced degradation studies enables identification of the degradation pathways of drug products and optimisation of their analytical methods to ensure they are stability-indicating.

Method Validation: Validation of analytical methods confirms their suitability for the intended purpose at different stages of product development. Partial validation is performed to support early-stage and clinical development. For later stage development, we conduct full method validation activities in accordance with regulatory guidelines.

Method Verification: PharmSky can perform method verification of compendial methods under the direction of a protocol with verification reports provided as required by the client.

Method Transfer: PharmSky works closely with clients to define the most appropriate approach for an efficient method transfer. Regulatory guidance combined with a risk analysis dictates the type of transfer, with the following transfer options typically considered: comparative testing, co-validation, re-validation and method verification.

Typical analytical methods that we develop and validate include:

• Assay/potency, impurities (degradation products/related substances for drug substances and drug products) methods
• Other physicochemical characterisation (e.g.colour, viscosity, density, water content, particulate matter, particle sizing) methods
• Cleaning methods for manufacturing process development
• Stability-indicating methods for API and drug product stability monitoring
• Residual solvents testing methods
• Comparator product characterisation methods

Based on the dosage, impurities of drug substances and drug products need to be assessed. If greater than the threshold defined in ICH Q3, an impurity must be structurally identified and characterised to ensure the safety and quality of the product.

Identifying unknown impurities can be a complex process that involves a combination of analytical techniques and expertise in chemistry. We undertake the following approaches for impurity isolation and identification:

• Identification threshold calculation based on daily dosage
• Isolation from the sample matrix by extraction or separation by semi-preparative HPLC
• Structural elucidation of the purified material using techniques such as NMR, mass spectrometry and IR spectroscopy

Stability testing provides evidence on how the quality of a drug substance or drug product changes with time under the influence of various environmental factors such as temperature, humidity, and light. PharmSky offers a comprehensive set of stability testing services that comply with ICH requirements, including:

• GMP stability programs
• Protocol preparation and program management
• Stability sample storage and management
• Stability testing of drug substances and drug products for clinical, registration and surveillance purposes
• Stability-indicating method development and validation
• Photostability and stress testing
• Extractables and leachables testing

Samples are analysed at different time points using appropriate methods to monitor changes in quality attributes such as potency, purity, and degradation products. The results of stability studies inform decisions regarding storage conditions, shelf life, and labelling requirements for pharmaceutical products.

• To develop/evaluate the stability-indicating nature of analytical methods
• To determine degradation pathways of drug substances and drug products to support formulation development
• To identify impurities related to drug substances or excipients

• Evaluation of solvents that are used in the manufacturing of a drug substance, drug product and/or an excipient.
• Residual solvent testing as per compendia methods.
• Residual solvent method development, validation, and verification.
• GMP release testing.