Has anyone dealt with moisture content analysis for lyophilized peptides?

Taking the question as asked, rather than the general version of it. The provenance questions are more useful than the numbers. Does the report name the batch on your vial. Is the date consistent with when that batch existed. Is it addressed to the vendor or to the person who paid for the test. Was the sample taken from general stock or supplied by the vendor. A perfect certificate for a different batch is worth nothing, and vendor-supplied samples are the most common way a genuine report ends up misleading.

LibrarianMeg said:

The provenance questions are more useful than the numbers.

That is correct as far as it goes, and here is where it stops going. One addition: an unstated method makes a report close to uninterpretable. "99% pure" without the technique, the standard and the conditions is a claim, not a measurement.

AttorneyGrant said:

I have a certificate reporting 99.2% purity and 6.1mg content on a vial sold as 5mg, and I cannot work out whether those two numbers are consistent or…

This matches mine closely enough to be worth saying so. Inter-laboratory variation comes from real methodological differences, not sloppiness: which reference standard was used and how it was itself calibrated, the gradient and column, the detection wavelength, and where the integration baseline was drawn. A percentage point or two between competent labs is expected. What is not expected is a large gap, and the usual explanation there is that one report is not of the batch in your hand.

Adding the clinical framing, because it changes how the question reads.

Mass spectrometry confirmation for certificates of analysis: beyond HPLC purity, mass spec tells you the molecule's exact molecular weight. This confirms identity — not just purity.

Why this matters: HPLC can show you a "pure" compound, but if it's pure of the WRONG compound, purity is meaningless. Mass spec at m/z 4113.58 Da confirms it's actually semaglutide. My Janoshik report includes both HPLC and mass spec.

If your testing provider only offers HPLC, consider upgrading to include mass spec for at least your first batch from a new vendor.