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METHOD DEVELOPMENT AND VALIDATION SERVICES

Pacific BioLabs has vast experience in analytical and bioanalytical method development, validation, and sample analysis - specializing in HPLC method development and validation. As both an in vivo and analytical CRO, we support product development of a variety of pharmaceuticals, biologics and medical devices.  Method development and validation is an important first step to determine that analytes of interest can be reliably detected and quantified during routine sample analysis. Our team of senior scientists and chemists will work with you to understand your product and development needs.  Based on our prior experience with similar products and by drawing upon published literature resources, we can develop the most appropriate method for your product.

After method development, we can validate the method according to FDA, USP, EP or ICH guidelines to determine its suitability for its intended use. We are flexible in supporting complete or partial validations, re-validations and method transfer. PBL provides full documentation including a transfer protocol, validation protocol, method, and a report generated with QA oversight.

Parameters Included in PBL's Validation Protocols

  • Accuracy
  • Repeatability/Reproducibility
  • Precision
  • Specificity/Selectivity
  • Limit of Detection (LOD)
  • Limit of Quantitation (LOQ)
  • Linearity
  • Range
  • Robustness
  • System Suitability
  • Sample Stability

Analytical Techniques Available

  • High Performance Liquid Chromatography (HPLC)
  • Liquid Chromatography/Tandem Mass Spectrometry (LC/MS)
  • Gas Chromatography /Mass Spectrometry (GC/MS) with headspace sampler
  • Inductively Coupled Plasma /Mass Spectrometry (ICP/MS)
  • Enzyme Linked Immuno Sorbent Assay (ELISA)
  • Instrumentation Details

For a complete list of our analytical instrumentation, click here.

Method Development Experience

Below is a case study that describes our team’s support for a client’s CMC study. It also highlights our team’s critical thinking and problem-solving approach, and their ability to think outside the box.

Case Study: Identification of an Unknown Impurity

Challenge

During a routine quality control check for lot release of their protein product, a biopharmaceutical maker saw a new peak on the SEC chromatogram. The Company had been manufacturing this Product for more than 5 years without any issues.
At first, the Company thought this peak was an amino acid which would indicate the Product had degraded. But no degradation products had been observed in the past 5 years. Thus it was possible that the peak was an impurity.

Our Solution

The Company approached the analytical team at Pacific BioLabs to solve this issue.

Our team repeated the QC check and of course, saw the same extraneous peak. We isolated and identified this peak as benzyl alcohol, thus confirming the Company’s suspicions that it was an external impurity.
Our team asked the Company if they had recently changed vendors for any materials used during manufacturing of the Product. Indeed, the Company had a new Supplier that made an ammonium sulfate salt, which was used to purify the Product.

Our team looked up the new Supplier’s website and found that the Supplier made both benzyl alcohol and ammonium sulfate at the same site! Even though the purification agent (ammonium sulfate) had been qualified per USP tests, it had been contaminated by benzyl alcohol. The contamination must have occurred because the manufacturing equiment had probably not been cleaned completely after the benzyl alcohol was made.

Conclusion

Our team concluded that the benzyl alcohol impurity was not detected by the USP qualification tests conducted by the Supplier because it was present in a very minute amount. But when the Product was concentrated during the purification step by the Company, the impurity was also concentrated along with it and therefore the new peak appeared on the QC chromatogram.

 
 
 
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