Analytical Method Challenge 1
Method Development and Validation of Challenging Drugs
A client came to Velesco with a peptide drug in preserved solution. The current analytical method was in use for the drug without preservative. The client needed a Phase 3 method to quantify both the drug and the preservative, with improved resolution of a closely eluting impurity and shorter run time.
The preservative was well separated in the current analytical method, but was over the maximum detection capacity. Also, several lots of commercially available preservative had an impurity that co-eluted with the active drug peak.
- Velesco developed a new HPLC method using an ion pair reagent that provided resolution of the preservative impurity from the active peak, improved resolution of the active impurity, and reduced the retention time by nine minutes.
- The preservative quantitation was successfully performed in the same run by using a second collection wavelength to bring the peak onto scale.
- Velesco performed the method validation for the two strengths of drug formulation.
During method validation, several new drug product strengths were introduced. Research data showed that the drug product could not be reliably quantified against a one-point standard curve to meet Phase 3 needs. In addition, the sample and standard matrix needed to match exactly for accurate quantitation.
- Velesco successfully re-validated this Phase 3 method for the new strengths of drug product using a matching standard for each sample.
- The matching standard contained equivalent preservative and excipient concentrations to the sample.
- All method validations passed Phase 3 requirements.
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