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ForumsCOA & Analytical TestingHow to commission independent testing — need advice

How to commission independent testing — need advice

wendy_avl Thu, May 2, 2024 at 11:19 PM 18 replies 2,066 viewsPage 1 of 4
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wendy_avl
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Oct 2024
Asheville, NC
May 2, 2024 at 11:19 PM#1

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

What I actually want to know is whether a purity figure and a content figure can disagree without one of them being wrong.

If the honest answer is that nobody knows, that is a useful answer and I would rather have it.

12 7SleepFixSam, PurityPaulOR, MaxMetOK and 9 others
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Dr.GastroMayo
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Mayo Clinic, MN
May 2, 2024 at 11:27 PM#2

Answering the narrow version, because the broad one does not have a single answer. 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.

11 6VendorMark, COA_Karl, MikeFit_NJ and 8 others
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BethLabQueen
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May 2, 2024 at 11:35 PM#3
Dr.GastroMayo said:
They are not contradictory, they measure different things, and this is the single most common misreading of a certificate.

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.

10 5lori_vegas, Dr.PulmRoch, maya_sedona and 7 others
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tampaLisa73
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Oct 2024
Tampa, FL
May 2, 2024 at 11:43 PM#4
wendy_avl said:
Two reports on the same product from two laboratories, four percentage points apart, and no method stated on either.

This matches mine closely enough to be worth saying so. 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.

9 4mike.trainer_LA, sarah_nash92, FitDadDave and 6 others
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LipidDoc_ATL
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May 3, 2024 at 12:23 AM#5

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

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: 99.6% purity
Day 14: 98.0% purity
Day 28: 97.0% 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.

8 3KristenIndy, MarkLI_maint, Dr.PeteFamMed and 5 others
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