A week ago I did an IPA extraction of 50 g of very finely ground black caapi from coon. To alleviate clogging I added 1&1/2 tablespoon of Diatomaceus Eearth (DE) to the caapi powder.

The powder was extracted for 5 hours in a homemade Continuous Solid-Liquid Extractor that is more efficient than a standard Soxhlet. At the end of the extraction the IPA, filtering through the plant material was completely colorless.

After distilling off most of the IPA I dried the extract until it has become a thick goo. Then I diluted the goo in phosphoric acid diluted to pH ~2.5. The solution has been left to settle for 12 hrs, then it was decanted and filtered. Then the solution has been basified with NaOH to pH ~13. Immediately white flakes started to form. In 8 hrs the precipitate settled completely. The precipitate has been washed with distilled H2O twice. Each time the solution was settled for ~8 hrs and decanted. Each time liquid was saved, but it did not produce any precipitate after 24 hrs of settling, so it was discarded.

The final solution had pH ~10. After decanting and drying the solids were weighed. The yield proved to be very disappointing - only 130 mg of light-brown powder (0.26%).

My questions:
1. Do you see any flaws in the above extraction procedure?
2. Does anybody have experience extracting caapi with alcohols, especially with Soxhlets.
3. Does anybody noticed negative effect of DE on yields in any extractions? In my experience DE noticeably reduces yields in spice extraction.

Of course, there is a question of the initial material quality, but I would like to exclude my own screw-ups first.

P.S. I still keep the sludge left from filtering my acidic solution.

I don't have much to add other then I'm guessing your DE did what adsorbents to best and adsorbed your target compounds. Hence the loss of yield.

50g of caapi ~ 250mg of alkaloids(ideally).

1-1.5tblspoons is probably several grams of adsorbent. 5 hours of 'soxhlet' is a lot of energy for such a small project. You're sure that your design of the extractor is sound? Are you putting the DE beneath the solid material so the solvent drips through it? Or is it mixed into the powder to aid flow?

I don't know much about soxhlets or continuous solid-liquid extractors. Just thought maybe I could help anyways...

Hmmm. After reading Gibran's "Easy tek" I expected close to 1 g from black caapi.



Yes. It has been used in many extractions. Usually it takes only 3 hrs to completely extract 50-70 g of mhrb. I ran it for 5 hrs because this was my first time caapi extraction with IPA. For extractions I use alcohols or DCM, so heat consumption is much less than with water. Using regulated heating mantle and sami-closed system also saves heat and solvents are not evapped into the environment.




DE was mixed into the powder.



Thanks.

Will ran similar extraction but without DE next time.

IPA is not a good solvent for harmalas, ive tested using it myself (not soxhlet though). If you want to go for alcohols, it seems methanol is better, followed by ethanol. Maybe if ethanol is a bit wet (gotta test different percentages.. starting with 96% maybe?) it will be good yields and yet not pull so any impurities.

What's wrong with acidified water? Isn't it more environmentally friendly, cheaper, takes around the same time(if not significantly less) and is sure-fire.

Wow 50g of caapi is giving people 1 gram yields now? Stuff must have evolved.

To extract caapi properly in traditional way it is necessary to do 3 cookings ~1 hr each + decanting of the liquid + reducing. Although gibran says that 3x30 min is enough, I do not think so.

Extractors are more efficient, otherwise ppl would not use them, but extractors tend to clog, especially if you use water in them, even more so if your plant material is fine powder. I have experimented a lot with water as extracting solvent and abandoned this route completely. Clogging, especially with fine powder, makes water unusable. Also water, as extracting solvent, requires much more heat. So, after a lot of experimentation I have settled for the following procedure (for spice):
1. Alcohol or DCM pre-extraction.
2. Discarding of solids.
3. Distilling the solvent. Usually I manage to recover up to 80% of it.
4. Drying the extract.
5. A/B extraction.
6. Hexane extraction.

It only looks complicated. Once you gain some experience the whole process 1-6 takes less than 8 hrs. I also think that the above process is more eco-friendly.


Yes. Check this - https://wiki.dmt-nexus.m...lkaloid_Extraction_Guide

Interesting. Will try later. Now, for the sake of good science, I will change only one parameter - will not use DE this time.



Yes, I've read that 70% methanol has been used by some researchers for caapi extraction. So, next time I will try different alcohols with different concentrations.
DCM is another interesting possibility.