Best Solvent Ratios for DCVC separation of THC and CBD?

Who has used DCVC to separate THC and CBD Class Cannabinoids? And would DCVC be a good choice for remediating 2-5% THC from a 60-80%CBD oil?

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Ask @Beaker, Hes got loads of experence with it !

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I would be interested in learning more also @Beaker

@beaker has lots of experience with DCVC, but I don’t know that he’s made any attempts to fractionate cannabinoids.

sure would be a neat trick though.

“The solvent system is generally Ethyl Acetate and Hexane starting with hexane alone. Then the Ethyl Acetate is added in 5% increments and is collected 20ml fractions at a time. Once the gradient is over about 30% Ethyl Acetate to hexane the majority of wanted fractions have eluted. Then I add Ethyl Acetate alone along with methanol to move the waxes and chlorophyls and just general gunk off the column.”

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I have never set up on compound with CBD or anytying elso than THC. I suspect DCVC as I practice it will do poorly using standard silica gel. Those molecules are very similar to each other and I would predict they travel about the same rate through a DCVC column.

Of course I am just one guy practicing one protocol. I find it useful to separate the half dozen or so color bands that go way slower in my column than THC. I have read unsubstantiated boasts that reverse phase media can separate the two. The deal about DCVC is it really is part art and part science. It can take a long time to nail down the procedure. Solvent systems are closely guarded secrets from what I gather but generally those reverse phase systems seem to hold the most promise.

I was offered an R&D spot in a group wishing to accomplish such separation. The problem is lack of data so my first priority will be to generate a boiling point curve and try to nail down exactly the differences if that is possible. I wonder if CBD represents just a fad for a newly emerged (from prohibition) industry? I find it interesting that now prohibition is over mostly that the drug most sought after seems to be CBD and not THC after all. Does this make CBD a gateway drug? lol.

CBD does seem to be easier to refine to high purity and I am hoping to work out just why that is and just how it might be leveraged. :nerd_face:

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Well correct me if I’m wrong, because I’m new to all this, but THC has 2 hydroxyl radial and CBD has 2 hydroxyl radial and 1 carboxail radial. So cbd will grab on first in the reverse phase dcvc due to the extra radial. Is this correct?

Is there any way to just convert THC without converting CBD? On a mass scale? Just an :bulb:. Then you wouldn’t have to remediate just react correct? This could save lots of time.

I’m located in portland Oregon rd now.
Please dm me for answers.

I have 97% cbd isolate with .27% CBN and .27% cbdv. To reciprocate for good information.

Thanks
Chris
I.g. Thirdcoastextractionscbd
541-227-3527 text first please

JMC Extractions - CBD Isolate CBN CBDV.pdf (202.8 KB)

I’ve been able to remove 85% of THC from crude using DCVC.

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@MyerP15

With reversed phase chromatography using methanol and water step-wise gradient, it takes about 20x the volume of material to be remediated in solvent.

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Details, please. What diameter is your column ?
Are you loading it according to Prof. Pedersen’s recommendation (0.5 g /cm^2) or more ?

are you refering to this video?

edit: yes you are!

if you havent watched this video, you should!

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Yes I am.
And yes, I have indeed watched it, and I’ve occasionally
done dcvc myself, but only with normal phase silica.

However I’m not daring enough to simply assume not much
else will change when swapping out one stationary phase
for another, so I’m asking :wink:

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If I am looking at the right molecules, I see CBD has two hydroxyl groups

THC has an ether group and one hydroxyl group.

I believe CBD is a little more polar because of the two hydroxyl groups.

When I ran reversed phase HPLC for cannabinoids, CBD eluted several minutes before THC, I suspect because the two hydroxyls on the CBD make it “want” to spend less time in the stationary phase. For that method I think the retention time for CBD was around 2.2 minutes (?) I don’t remember exactly.

Reversed phase method was acidified methanol water (82/18), 4.6 x 150 mm ARC18 column from Restek. I think the runtime was 7 mins.

Never did any normal phase separations

image

Yes you are correct @anon81723932 the cbd - thc separation is a relatively easy one
with rp silica.

However the difference between analytical and preparative separation is easily eight
or so orders of magnitude. You’re injecting, say, 10 nano grams into the raptor, but
you want to do the same separation in your production lab on a kg scale…

That’s a similar ratio as one gram (as in one pipette full of tincture) in comparison
with a sizable swimmg pool.

By and large, the same rules still apply, and yes, the method should be transferable.
However, at the same time you also need to improve it, use the least amount of
solvent, highest loading, substitute AN with (cheaper) methanol etc., in short,
optimize the method for lowest cost/time/manual labor.

If anyone has done that yet, please speak up and share :slight_smile:

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In the meantime, for everybody’s enjoyment, here’s a related graphic from Restekall-16.pdf (100.5 KB)

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