Method development & validation

Analytical method development

The development process can take various forms although typically includes a number of common stages from initial concept through to investigative analytical testing. The overall process length is largely dependent on the complexity of analyte, sample matrix, method goals and potential analytical target profile (ATP) requirements. Importantly, ALS considers the environmental impacts of analytical development and proactively seeks ways to reduce a methods carbon footprint wherever possible. ALS strive to develop well-tuned, risk adverse and lean analytical methods in support of lifecycle management and readiness for ICH method validation.

ALS can support isolated part of development or own the process as whole inclusive of validation:

• Background Research
• Developmental Process Design
• Risk Assessments
• Analytical Technique Selection
• Proof of concept work
• Determination of analytical conditions
• Stability indicating assessments
• Analytical Troubleshooting
• Method Optimization

Common projects include:

• Development in support of New Product Launches
• Adaption of compendia methods to alternative product dosage forms
• Method Screening across different column chemistry
• Transference from reverse phase HPLC to UPLC
• Application and implementation of newer analytical technologies
• Method consolidation

Analytical method validation & verification

ALS regularly supports the validation of various analytical procedures from simple identification tests through to more complex, stability indicating quantitative testing techniques per ICH Q2 guidelines, USP <1225> and client driven needs. The increased focus on lifecycle management of analytical procedures, where ICH Q8 can be adapted, naturally leads ALS to developing and validating methods by applying Quality by Design (QbD) concepts and using analytical target profiles (ATP) as appropriate. Traditional ICH validation characteristics can be supported by a framework that allows users to reliably understand and control sources of variability. An effective Analytical Control Strategy supports both Quality Risk Management and Knowledge Management together.

Typical validation characteristics include:

• Accuracy
• Precision
• Repeatability
• Intermediate Precision
• Specificity
• Detection Limit
• Quantitation Limit
• Linearity
• Range
• Robustness
• Filter Studies
• Establishment of solution stability

A broad laboratory network gives ALS clients access to advantageous inter-laboratory transfers, inter-laboratory verifications and heighted but controlled challenges to the real-world risks often overlooked within the robustness validation characteristic.

Analytical method transfer

Analytical method transfer (AMT) is formal process for the introduction of new methods which allows the receiving laboratory to demonstrate that they can perform the analytical method effectively and reproducibly. Effective protocols should consider all critical quality attributes and method parameters with a view to maintain the method's validated state and support continued procedure performance verification.

Our facilities support transfers in a number of ways, typically by performing comparative testing, compendia verification or re-validation as broadly described within various regulatory guidelines and USP <1224>. Identified validation gaps can be filled as part of transfer activity. Each method of analysis, specification and method transfer protocol undergo a thorough technical review before the commencement of transfer activity. ALS can assume varying degrees of responsibility, at the direction of its clients, from protocol writing, material procurement, risk assessments to final reports and transfer and training into other Quality Control Laboratories. All transfers are conducted in an open and collaborative manner with quality, regulatory requirements and ultimately patients in mind.