Hi, we are seeing CBD distillate sometimes eluting as CBDA on our Agilent HPLC. I noticed this last batch we ran was the most acrid smelling run we’ve had. Process is cold ethanol extraction, filtration, solvent recovery in a Pinnacle SRS, finish and activate the oil in rotovaps that have silicone heat fluid (135-140C). Distillation is an IPS 2 stage WFE. Residue stream shows CBD but distillate shows nearly pure CBDA.
Thoughts?
Thanks!
Bump!
How long did you decarb for? At that temperature you’re practically guaranteed to get all of the CBDA out. What kind of calibration are you performing on your instrument? Do you recalibrate the curve every month? Do you PV every day? Have you tested an old batch that you read as CBD to see if it still reads as CBD?
Distillate shows nearly pure CBDA??
That’s very interesting. My initial thought was HPLC error, maybe a random shift in retention time for this particular injection. How long do you rotovap decarb for? Also interested in your WFE parameters if you are able to share them.
What does your calibration CCV look like? When’s the last time fresh mobile phase was prepped?
What potency does your HPLC say your CBDA is? What vacuum does your WFE pull at? An easy test to see if it actually potentially is CBDA, take 1g of the distillate and heat on a hot plate to 140 - any CO2 evolution? Not sure if you’re in the position to waste 1g of material. If not gas evolves there might’ve been an issue with the HPLC
did you try decarbing at temperature and re-running sample? If it really was CBDA it would decarb when heated
I was curious if you could successfully decarb in a Roto vap and skip the oven all together.
At 140 degrees you may not unless you’re pulling a vacuum. I’m not sure tho.