Steam distilling virola resin?

[Nathanial.Dread]

I'm thinking in investing in some v. theiodora resin, but I'm not 100% sure what one can do with it. If there is DMT or 5-MeO in there, it seems like smoking, insufflating, and other common RoAs don't work.

Would steam distillation work to get the actives out, and then a liquid-liquid extraction with some kind of volatile organic solvent?

Alternately, could a Soxhlet apparatus work?

Blessings
~ND

 

[pitubo]

AFAIK virola material needs to be extracted when fresh or else it will lose potency. I wouldn't invest too eagerly in large amounts of commercial resin before establishing that it actually contains a reasonable amount of actives in the first place.

Concerning extraction of actives from resin, how about digesting it with dilute acetic acid, basing and extracting with a non-polar solvent like toluene? Then evaporate the solvent or precipitate fumarates with FASA or FASI.

If the resin will not readily yield to polar solvents like dilute acetic, you could start to dissolve in ethanol and dilute that with vinegar and subsequently boil off the ethanol until left with a solution of acetates of any actives present, in dilute acetic acid, and possibly a precipitate of insoluble inactives, which could be filtered or decanted. Don't do this boiling down inside closed and inadequately vented spaces, because ethanol is somewhat toxic and quite flammable and the acetic acid, that will inevitably also evaporate in substantial quantity, irritates and stinks. Availability and proper use of distillation glassware may mitigate some of these issues.

I have never heard about dmt or 5-meo-dmt being steam volatile.

Neither do I think that a soxhlet apparatus is particularly practical for extracting resinous material, especially if said resinous material is a liquid, however thick or viscous. A soxhlet extraction seems to be best suited to substances embedded in a solid, non-soluble and to a large degree porous or at least permeable matrix.

 

[Mindlusion]

Actually, soxhlet extractor is ideal for extraction of resinous materials. In pretty much every case you want to do an alcohol extraction, soxhlet is the way to go, you can always be sure you are extracting every last bit of the plant material. The resin won't be thick or viscous when its dissolved in the ethanol.

If your material is really too gunky and you are worried it will clog the soxhlet, you can grind it up first with some celite, or diatomaceous earth. This will keep it together so solvent can freely flow through it. Also helps as a filter too. Heck, better yet since we want to extract alkaloids, mix it up with some dry lime ala 69ron. That would be ideal.

Steam distillation might work too, but yields would be lower. The freebase would likely come over with other essential oils present in the resin. That is, if there is any in there. Would be fun to try, distilling essential oils is fun.

Though pitubo is right, getting virola with alkaloids in it is the issue. Still, worthwhile to try.

 

[pitubo]

A soxhlet apparatus can be useful to extract a resin from a plant matrix, but I was assuming that the virola resin is acquired already extracted and in a more or less liquid form. In that condition, it would be useless in a soxhlet. But mixing it with lime and putting that in a soxhlet for ethanol extraction might be an interesting approach, however I wonder if it would lead to any useful purification or if it would just be stripped back off the lime.

I have experienced freebase dmt co-distilling with heavier naphtha fractions, but I have doubts if it would do the same with steam. Moreover, the alkaloids in the resin are probably present in salt form, making steam distillation even more unlikely - apart from the issue of separating and recovering the alkaloids from the condensed steam.

If you have virola plant material, then yes, ethanol in a soxhlet sounds like a good way to get any actives out of the bulk. But you would end up with lots of other plant compounds, because the ethanol extraction is not very selective and the end result is a resinous substance.

 

[Mindlusion]

Yes this is true, would be rather pointless to extract an already extracted resin, I was assuming plant material. It was my understanding that 'virola resin' was not extracted but scrapped from the underside the of bark, a sappy rosin like material.

Non selective yes, but for plant material, absolutely, it reduces the amount of material you need to work with, as well as making it easier to digest in acid if you want to do an acid base extraction.

Freebase dmt co-distilling with naphtha, that is very interesting! I wouldn't doubt it with these alkaloids having low melting points, which also makes them very favorable for steam distillation as well, even alkaloids with fairly high m.p. can steam distill if they have a high enough v.p. or are prone to sublimation. Another thing you could do is steam distill with a co-solvent like toluene (steam azeotrope 80C or so) or naphtha. It could increase the amount of alkaloids that co-distill, or it could do the opposite too, who knows. And yes, of course the alkaloids need to be in freebase form first :d I doubt the salts would come over at all, unless the water was 'misting' they need to be non-polar to form the azeotrope and steam distill

These kind of techniques are more suited towards extraction of non-alkaloid natural products, and are not really any more useful for extraction of the alkaloids than acid base. It would be wise to first test the resin for content of 5-meo-DMT, then have a go at extraction. TLC of the crude resin may work well enough.

 

[downwardsfromzero]

Freebase DMT does indeed co-distil with heavy naphtha. This may conceivably be of some use in removing it from a resin matrix, except that if one has access to decent distillation gear one could probably come up with a better method as well :?

1ce was doing some stuff with co-distillation a while back.