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.

MikeFit_NJ said:

The provenance questions are more useful than the numbers.

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.

newstart_MO 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…

Same position here, arrived at the long way round. 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.

From the other side of the consultation, briefly.

I tested my certificates of analysis batch through Janoshik — 97.0% purity. That's within acceptable range for compounded peptides. Turnaround was 14 business days.

The test costs ~$126 but gives you actual HPLC chromatography data plus mass spec confirmation. For the peace of mind alone, it's worth every penny. I test every new batch from a new vendor.