Analytical Development and Validation Development Services

For early phase projects, we develop analytical methods in hand-in-hand with the process development program. For critical quality attributes of the final product such as assay, related substances, and residual solvents analytical methods are verified. Our standard analytical method verification procedures check LOD, LOQ, linearity, precision, specificity, accuracy, robustness, solution stability and mobile phase stability. Along with these verifications, fit-for-purpose analytical methods for testing raw materials, in-process controls, and intermediate analysis are developed. Post mapping of equipment at the manufacturing facility, an appropriate residue method is also developed and validated. We generate and qualify the appropriate quantity of reference standards to support the analysis and method transfers.

Typical characterization of the reference standard includes

• Characterization with appropriate spectroscopic techniques, Mass spectrometry, NMR and FT-IR
• Testing for its impurities (related substances or chromatographic purity) as per the pre-defined test procedure
• Water by KF or loss on drying
• Other parameters such as sulphated ash or residue on ignition (ROI) or residual solvents
• Determination of the potency of the reference standard
• The polymorphic characteristics of the material will be analyzed if it is a specific polymorph

We perform method validation as per the internal SOP of Aurigene against the predefined specification. The method will be validated as per ICH guidelines for parameters like LOD, LOQ, linearity, repeatability, recovery, solution stability, specificity, precision, accuracy, robustness and mobile phase stability. Analytical activities also depend on whether we are working on intermediates, RSM or the final API.

• RSMs - Analytical methods will be developed for the Regulatory Starting Materials (RSMs) and those methods will be validated. The key tests for the KSM would be related substances, assay and residual solvents along with the general tests such as appearance, Identification, water content, etc.
• For Intermediates - For the process validation campaign, analytical method validation for the intermediate stages required was followed by formal method transfer to the quality control site. Hence, we perform the complete method validation against predefined specifications and protocol and a report shall be created as per internal SOPs.
• For API - Analytical methods for the final API step would be validated before the start of manufacturing batches.

We also do the following analytical activities

• Forced degradation study - Specificity of the analytical test procedure will be demonstrated by various stress studies for the final compound in line with ICH guidelines by subjecting the sample to acid, base, peroxide, thermal, and photolytic degradation conditions, and a separate report will be generated for the forced degradation studies.
• Verification for pharmacopeia methods shall be done for identification tests like 1H NMR, 13C NMR, FT-IR, PXRD, DSC test, and water content by KF to confirm the identity test.
• Post mapping of equipment train at the manufacturing facility, appropriate residue method will be developed and validated.
• To support the analysis and method transfers, an appropriate quantity of the reference standard would be generated and qualified.
• Developing sensitive analytical methodology for Potential Genotoxic Impurities (PGI), Nitrosamines, Elemental impurities etc.
• Typical characterization of the reference standard includes:
  • Characterization with appropriate spectroscopic techniques, Mass, NMR, and FT-IR
  • Testing for its impurities (related substances or chromatographic purity) as per the pre-defined test procedure
  • Water by KF or loss on drying
  • Other parameters such as sulfated ash or residue on ignition (ROI) or residual solvents
  • Determination of the potency of the reference standard
  • The polymorphic characteristics of the material will be analyzed if it is a specific polymorph

We perform analytical validation in compliance with the Pharmacopoeia, current Good Manufacturing Practices (cGMP) and ICH requirements as per customer needs. Following are the salient features of our method validation activities:

• Method validation executed as per the well-defined phase appropriate SOPs which are in line with the current regulatory, ICH guidelines in accordance to cGMP requirements
• Our method validation capability includes KSMs, intermediates, APIs and drug product. SOPs are well defined to suit the phase specification method validation requirements
• Custom-field calculations, e-sign off procedures are enabled for chromatographic instruments to ensure the highest level of compliance.
• Validation activities recorded in to electronic lab notebook enforces online documentation in accordance to principles of ALCOA+
• Completion of validation to meeting stringent timelines
• Method transfer to QC

Stability studies:

We perform stability studies for developmental APIs, intermediates, RSMs and drug products.

• Stability studies as per ICH – Long term, Intermediate and Accelerated condition
• Short term temperature exposure studies
• Photo stability studies

We have the stability chambers, refrigerator and deep fridge storage suiting to requirements of different climatic zone.