Related industries have formal processes around testing, COAs, and verification. Sellers always sell/ship with a COA, buyers quarantine product while QA/QC verifies the COA through more testing, and material is not released (or paid for in many cases) until the verification matches the original COA and identity is confirmed.
Until the entire industry follows similar protocols together and such norms develop, we will continue to see companies skip these steps to undercut competitors on speed and cost. The sad outcome of this is that the market gets overwhelmed with poor quality products.
This is how it has to be done with rec cannabis testing in OR (and CA I think too) … Lab has to come sample the batch from the production site. Or the producer has to bring the entire batch to the lab for a proper sampling. In no way is the producer trusted to provide representative samples of the batch.
Never trust, always verify… Good motto to live by when dealing with something that is only like 5 years removed from the black market.
Why is HPLC testing a waste if the lab shows the chromatograms when I ask and each time the peaks are extremely and clearly separated between D8 and D9?
Is there some reason I can’t trust an HPLC chromatogram that has clear separation?
Are you saying the separation will be even more resolved if GC is used instead?
And how can MS help if D8 and D9 have the same weight?
I guess I am wishing that there is a “For 5-year olds” explanation of why GCMS is so important to proper D8 testing when, every time I ask the lab for a chromatogram on a D8 product COA, the resolution always looks great. Unless someone can tell me why I should ignore a great looking chromatogram, it is difficult to digest the idea that all these labs that have some kind of special sauce on their D8 testing have anything to offer at all other than perhaps interesting research.
The CBD isomerization reaction creates D9 and D8 via one pathway and the iso-THC compounds on a separate pathway. D4,8-iso-THC coelutes with D9-THC and D8-iso-THC coleutes with D8 on reverse phase HPLC. Inflated concentrations are easily reported, including a higher D9 value. On methods with poor separation four analytes can look like one, typically D8 since it’s highest in concentration.
GC and normal phase HPLC can achieve separation between all four compounds, so that they are quantified separately from each other.
We use triple quadrupole mass spec, which allows for fragmentation to be used in characterizing a compound.
What do you estimate as a great resolution ?
Could you show some example please ?
I believe FID is sufficient for this work.
MS brings a little more confidence in the fact that the analytes are THCs (or something that weigh and fragment similarly…) and not something totally different.
main fragment of d8 is 231, main fragment of d9 is 299.
however, the ‘unknown’ byproducts of the rxn have some fragmentation patterns that aren’t in any literature I was able to find. and I looked everywhere.
the most interesting ones are those that had a primary fragment at 277. I assumed this was the isopropyl group blasting off of the iso-THC’s, but since the standards of those don’t really exist (@kcalabs any update on standard procurement for these?) it was more guesswork and less validation from the literature
since I’m no longer pursuing the project, could you tell me what cannabinoids that you all have ‘discovered’ with a primary fragment at 277 m/z? i’m really just interested in why/how the structure would fragment that way!