Let’s start the conversation on cleaning up D8. I have ran lots of experiments best I got is 3%. RP on c18 seems unusable. Doing some NP with hexane and ether.
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What was your starting composition? You might want to look here for preprocessing:
After all, smaller d9 peak makes for less peak overlap
We ran a batch of isolate 98+ and distillate at 86%.
Started method development on RP but not having luck with it
I guess my question was if you had analytics on the oil post-reaction pre-cleanup. If you’re starting with 30% d9 it’s obviously going to be much harder to separate than 5%.
It seems like a lot of the analytical RP methods are using formic for pH adjustment which may be undesirable for a prep process
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I think these modes are restricted to HPLC but have you looked into chiral resins or functionalized crown ether resins? Those resins are more specialized for difficult separations. Even saccharide based columns might achieve better resolution https://doi.org/10.1016/j.chroma.2020.461256
Chiral was next on the list I have heard it does well with isomers. Got some on order
Have you run any TLC plates with varying solvent ratios to see what ratio may gave the best separation?
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I have not done any thc. I was hoping I could do it on a 69g column and scale from there
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Run TLC with 5% Ether 95% pet ether
On standard silica
Use a 1:50 ratio to begin with of disty or oil to silica and you’ll be where you need to be
You won’t need more than 4 column volumns of that gradiant then flush with etoh and re equilibriate for your next run or next pass depends how hot your d8 is going in on whether you need 2 passes or 1.
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Use an adsorbant media packed into wide and squat “pancake” column, that adheres the thc and rinses the impurities, wide and flat ensures lots of surface area for your mobile phase to rinse and remove the non-THC elements from the system- and that the cannabinoids don’t clog your column- elute the cleaned off cannabinoids with a strong solvent and recover
Easy, straightforward, and absolutely able to be accomplished via the remediation media available via @GreenMachine_Consult
It could not be any easier or more straightforward,
DM for details.
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Run TLC to figure out optimal solvent for best separation. Ifs cheaper than actually running columns via trial and error to figure out best separation. You can use Rf value to help determine optimal mobile phase composition. Once you have developed the mobile phase with TLC, then run your column
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Loser!