Method Development & Validation Services
Method Development and Validation
The US FDA requires that pharmaceutical companies ensure the identity, strength, quality, purity, and potency of the drug substance and drug product being marketed. Analytical test methods used for these measurements must be validated for both NDA and ANDA products. Analytical method validation is also required for some compounded pharmaceutical products.
Vici Health Sciences offers analytical method development and validation as a stand-alone service or as part of a full product development package. Being a full service, end-to-end product development CDMO, we are experts in all aspects of HPLC analytical method development, testing, and validation. We perform ID, assay, dissolution, impurity, content uniformity method development and validation, and can guide your overall program with meticulous troubleshooting when necessary. Vici is your one-stop R&D experience.
Analytical Method Development
Analytical methods must be developed for a specific drug product to be developed or manufactured. Compendial methods such as USP drug product methods, when available, drug substance methods, or literature-based methods do not work for all products due to varying strengths, inactive ingredients, and manufacturing technologies used. Vici will develop analytical test methods for each specific drug product to ensure FDA compliance and quality.
What is analytical method validation?
The International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH) in conjunction with regulatory agencies including the Food & Drug Administration (FDA) provide detailed guidance on the requirements for analytical method validation of pharmaceutical products. The guidance document ICH Q2(R1) is considered the primary reference for recommendations and definitions on validation characteristics for analytical procedures. Typical validation characteristics include:
- Specificity/Selectivity
- Range
- Accuracy
- Precision
- Robustness
- Specificity
- Accuracy
- Precision
- Range
- Quantitation limit
- Detection limit
Stability-indicating analytical methods
If an analytical test method can detect changes in the quality attribute(s) of the drug substance and drug product during storage, it is considered a stability indicating test. To demonstrate specificity of a stability-indicating test, analytical chemists typically use samples spiked with target analytes and all known interferences, samples that have undergone various laboratory stress conditions, and actual product samples (produced by the final manufacturing process) that have been stored under accelerated stability conditions or otherwise aged. A stability indicating assay method must be able to distinguish between the drug substance or active ingredient HPLC peak and degradant peaks to ensure that the correct assay or potency is measured during stability studies.
Drug substance analytical test methods
Compendial methods or methods developed and validated by drug substance (API) vendors can be used for drug substances upon completion of method verification or method transfer. In cases where drug substance manufacturers do not provide validated stability-indicating methods, Vici can develop such methods de novo.
When is method validation required?
All analytical test methods must be fully validated prior to releasing phase 3 clinical material, formal stability/registration batches, and for NDA or ANDA filing. Analytical test methods must be fully validated for testing commercial batches and for tech transfer of approved batches.
Full method validation is not required early-stage formulation development. Phase appropriate analytical method qualification or validation is sufficient for early phase clinical batch release (such as phase 1 or phase 2 clinical trial batch manufacturing release testing and stability). However, the use of R&D methods that are not qualified or validated appropriately cannot be used.
Full analytical method validation is not needed when validation is performed at a third-party site and the methods are transferred into the receiving lab for further testing.
Is analytical method validation for clinical trial material the same for commercial product?
The FDA utilizes the concept of phase appropriate method validation. This concept focuses on patient safety with increasing stringency as the clinical program goes from early to later stages of FDA approval and commercial manufacturing. Vici Health Sciences is well versed in this concept and can guide you through the specific requirements at each stage of your program, saving you time and money.
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