CBD nucleation - precipitation under terpene supersaturation

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1

Has anybody tried this?

I have to crystallize some CBD for r&d and i am not allowed to use Pentane here.

Was wondering if anybody had successful results precipitating it using Pinene or similar and if so, what were your results? Were you able to crash up to 50-60% of the total content?

Thanks!

2

Using non-native terpenes would likely be your best bet, the fractions from the plant are good at keeping it dissolved. I’m sure there’s an isolate that would be relatively ideal.

Can you not use heptane either? Generally, even in strictly regulated areas heptane is allowed.

3

Heptane and Hexane also work very well if that is an option.

4

I tried this with limonene and it didn’t work

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5

CBD will readily crystallize at a high enough percentage. What purity/potency are you looking at? If pentane is not allowed, heptane and hexane also work.

6

Thanks everyone for the reply. I have a 1ppm allowed residual solvent for hexane (which might make it difficult, specially with Potential solvent trapped in the crystals), but i will check for heptanes, maybe i have better luck.
Did you encounter any difficulties removing the heptanes residue? Were you able to have a decent yield?

Thanks

7

below 1ppm is going to be very hard for any isolate and any solvent. Most labs have a LOQ higher than that though.

I would start by asking the lab you plan to use what their LOQ and LOD is for hexane an heptane and use that answer to decide what solvent to use.

8

That’s a good idea. I’ll find out their llod and lloq.
EU is tough.

I was thinking of maybe micronizing the isolate and placing it in vac oven on thin layer or in a reactor with agitation to try and pull those residues. Can’t really say if it would be successful

9

Would you use a similar supersaturation ratio with Heptanes that you would with Pentane?

If you don’t mind sharing, did you also work a nucleation curve with temp/pressure parameters?

Thanks.

10

I personally have never used heptane to crystallize, I just know its a very common solvent to use and works similar to hexane. when I use hexane its 1.5-2 time the volume to weight of oil.

Ie. 1000g distillate to 1500-2000ml solvent.