Chromatography Forum

Hi,

I am working on a few new methods to quantify processing residuals in final products. Things like solvents etc.

Normally, we work within the FDA specification (ORA Lab Manual Vol. II - Methods, Method Verification and Validation (ORA-
LAB.5.4.5)) of 97-103% for APIs and 95-105% for final dosage forms. But a residual solvent is neither an API or final dosage form.

I'm seeing a general acceptance criteria of 80-120% for accuracy %recovery during method validation, but I can't seem to find a concrete source for this. I'd like to not have to develop new methods to a stricter requirement than necessary, but without a reliable source I don't see how I can justify the 80-120% range.

Would really appreciate if anybody with more experience/knowledge in this area could provide some input please.

Normally, we work within the FDA specification (ORA Lab Manual Vol. II - Methods, Method Verification and Validation (ORA-
LAB.5.4.5)) of 97-103% for APIs and 95-105% for final dosage forms. But a residual solvent is neither an API or final dosage form.

The company I worked for did not make APIs; we bought APIs and put into a final dosage product. Your post reminds me of the time I had to ARGUE from same ORA source with our QA Director to get him to accept the 95-105% range (he wanted 98-102% which we almost always met, but I felt for our topical products it was ridiculous to have tighter standards than the FDA).
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But a residual solvent is neither an API or final dosage form.

I'm seeing a general acceptance criteria of 80-120% for accuracy %recovery during method validation, but I can't seem to find a concrete source for this. I'd like to not have to develop new methods to a stricter requirement than necessary, but without a reliable source I don't see how I can justify the 80-120% range.

Would really appreciate if anybody with more experience/knowledge in this area could provide some input please.

Another time I had a method for an "impurity" that I wanted to do a validation for; the best I could find was from Australian Veterinary publication, title page and page 3 attached below. This showed different %Recovery guidelines depending on the level of such impurity. There may be newer information out there. Our QA Director looked down on this publication because it was Veterinary; there were other, and multiple reasons I believed this QA Director was not competent.


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