Test Method Validation Help - New titration test method, not defined in the USP

[SarahRYMoore]

I am relatively new to the pharmaceutical industry. Our lab is in the midst of developing a new titration test method, not defined in the USP. What kind of information should we include in the test method validation protocol/report? We have currently set up the testing to look at 3 different concentrations across a typical range, using 2 operators and 3 trials of each test. I am very familiar with Gage R&R studies, but the requirements on this type of test method validation seem less defined. Further, I am limited in resources to Excel. I used to work for a company that used Minitab. Those were the days! Any help anyone has is so much appreciated. Worksheets, tables, references, suggestions, guidance...I appreciate it all.

Thanks,
Sarah

[Marc]

Anyone here familiar with titration tests?

[chiragtilara]

A Typical Method Validation in pharmaceutical industry includes:

1. Accuracy studies - (generally done when extraction or recovery is an issue). This may be required if your analyte is extracted into titration medium

2. Linearity - to make sure that range you wish to operate your test has a linear response.

3. Repeatability and Reproducibility - Also covers intermediate precision - generally done repeated by operators. - Your GageR &R should cover this requirement.

4. Limit of Quantitation/Detection - Generally done for chromatographic methods. - this is basically done to ensure that your method has a strong response (compared to noise) at low levels of analyte.

HTH

-CMT