Particulate matter testing — USP <788> for injectable peptides

CarlaRPh_TPA said:

The provenance questions are more useful than the numbers.

My HPLC chromatogram analysis for certificates of analysis — I sent my batch to Janoshik and here's what the results showed:

Main peak retention time: 16.3 minutes (consistent with semaglutide reference standard)
Peak purity: 99.8%
Related substances: 0.6% (single impurity at 10.7 minutes — likely a synthesis intermediate)
Mass spec: m/z 4113.5 (matches expected molecular weight)

This is a clean result. The mass spec confirmation is particularly important — it proves the molecule is actually semaglutide and not a substitution.

A narrower follow-up, since the general answer is now clear:

Whether a purity figure and a content figure can disagree without one of them being wrong?

jason_paloalto said:

My HPLC chromatogram analysis for certificates of analysis — I sent my batch to Janoshik and here's what the results showed: Main peak retention time:…

Reconstituted peptide stability data for certificates of analysis: I had Janoshik test my reconstituted vial at day 1, day 14, and day 28 stored in the refrigerator.

Day 1: 99.4% purity
Day 14: 98.0% purity
Day 28: 98.4% purity

Minimal degradation over 28 days when properly refrigerated. This confirms the standard 28-day beyond-use date is appropriate. Beyond 28 days, I'd reconstitute a fresh vial to be safe.

Closing the loop on my own question.

Purity and content being different measurements was the piece I was missing. The vial was overfilled and pure, which is a very different problem from the one I thought I had.

Dr.NephBHM_UK said:

Reconstituted peptide stability data for certificates of analysis: I had Janoshik test my reconstituted vial at day 1, day 14, and day 28 stored in…

Agreed, and mass spec answers a question purity does not: identity. High purity tells you one thing dominates the chromatogram, not that it is the molecule you ordered. A mass within about a dalton of expected is the identity check.