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ForumsCOA & Analytical TestingCommunity-funded testing initiative — 6 month update

Community-funded testing initiative — 6 month update

Dr.RheumBOS Sun, Aug 4, 2024 at 3:53 PM 11 replies 1,876 viewsPage 1 of 3
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Dr.RheumBOS
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Aug 4, 2024 at 3:53 PM#1

Two reports on the same product from two laboratories, four percentage points apart, and no method stated on either.

The narrow version of the question is whether a purity figure and a content figure can disagree without one of them being wrong.

Numbers rather than impressions, if you have them.

23 18pam_stl, wei_SG, cory_ATX and 20 others
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InsuranceTom
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Aug 4, 2024 at 4:08 PM#2

Short answer first, then the reasoning. 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.

Last edited: Aug 4, 2024 at 9:08 PM
22 17lucas_SP_BR, lisa_labSD, adam_van and 19 others
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MounjBrad
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Aug 4, 2024 at 4:23 PM#3
InsuranceTom said:
Inter-laboratory variation comes from real methodological differences, not sloppiness: which reference standard was used and how it was itself…

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.

If somebody has the primary source to hand I would rather cite it than paraphrase it.

Last edited: Aug 4, 2024 at 9:23 PM
21 16nick_SD_fit, ben_calgary, patPC_UT and 18 others
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Sigma-Aldrich — Research-Grade Standards

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ChrisMacros
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Aug 4, 2024 at 4:38 PM#4
Dr.RheumBOS said:
Two reports on the same product from two laboratories, four percentage points apart, and no method stated on either.

Can confirm the pattern Dr.RheumBOS describes. They are not contradictory, they measure different things, and this is the single most common misreading of a certificate. Purity is a relative area measurement: the main peak as a percentage of total peak area in the chromatogram. Content is an absolute mass measurement against a reference standard. A vial can be 99% pure and contain 6.1mg — pure material, overfilled — or 99% pure and contain 3mg, which is pure material and a short fill. Purity tells you what fraction of what is there is the right molecule; content tells you how much of it there is. You need both, and a certificate with only purity is telling you half the story.

If somebody has the primary source to hand I would rather cite it than paraphrase it.

Last edited: Aug 4, 2024 at 7:38 PM
20 15LibrarianMeg, bri_stats, pete_manc_UK and 17 others
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NurseAsh_DET
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Aug 4, 2024 at 5:59 PM#5

From the other side of the consultation, briefly.

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: 15.4 minutes (consistent with semaglutide reference standard)
Peak purity: 99.1%
Related substances: 0.8% (single impurity at 9.5 minutes — likely a synthesis intermediate)
Mass spec: m/z 4113.6 (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.

19 14emily_PDX, Dr.SleepRoch, laura_annarbor and 16 others
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