When approaching a Banisteriopsis Caapi extraction there were several things to consider.

The most sought after alkaloid THH (Tetrahydroharmine) has been theorized to not even get extracted during a typical Manske extraction.

Additionally, the whole point of doing the Manske is to separate out the toxic compounds in Rue. Caapi has no toxic compounds and there is no worry of cross contamination.

The Herbal Percolator (Featured Here) has been said to make Caapi active at doses as low as 10g! That means it must be extracting much more efficiently. The grams of material to water ratio is 1g:150ml so that means 37,500ml or roughly 10 gallons.

This approach did an acid extraction using The Herbal Percolator. Instead of adding salt, the alkaloids were freebased DIRECTLY out of the acid solutions, pulling the full-spectrum of caapi compounds.

The approach utilizes the Homemade Pressure Pump, Found Here.

Procedure:

1. 250g B. Caapi was chopped & then powderized in a coffee grinder.
2. The Caapi powder\shreds were setup in The Herbal Percolator.
3. 10 gallons of near-boiling vinegar water was run through the Percolator.
Note: About 1/2 cups of Vinegar was added for every 4 cups of Water after the water was taken off the heat
4. The 10 gallons was reduced down to 1 quart
5. The solution was refrigerated overnight to decant
6. In the morning the solution was ran through a cotton filter
7. The solution was then run through the Pressure Pump
Note: Several coffee filters got clogged and replaced at this point
8. The solution was warmed
9. 3 big tablespoons of Sodium Carbonate were added to fresh water and mixed well
Note: Cook baking soda in the oven @ 420F for 3 hours to produce Sodium Carbonate
10. The Sodium Carbonate concentrated water was filtered through a cotton filter to remove excess
11. The 200ml concentrated Sodium Carbonate solution was poured into the Caapi solution
Note: The color rapidly changed but reached equilibrium by the time all was added
12. The solution was left to settle for 2 hours in the fridge
13. The solution was filtered through the Pressure Pump
Note: This step used about 8 coffee filters, all soaked in a thick coat of alkaloids
14. All the coffee filters used through the pressure pump now had thick 'cakes' of Caapi alkaloids
15. The coffee filters were dried in a food dehydrator set to 115F

Tips:

-Make 2 Herbal Percolators and put 125g in each one. This will make the whole process go a LOT faster. Use 5 gallons of water per percolator.

That's it! 8.2g Crude Caapi Extract!

Normally some would be left as-is for experimenting, this crude extract looks AMAZING! For the sake of the extraction all of it will be purified to see how much it yields of clean goodness.

Quite impressive work there! I like how the final product looks like chocolate scrapings! Its very interesting also that when one dries with vacuum (or positive pressure in your case) the product seems to come into a cake/flakes. I really recomend such methods of filtering ,it seems to make the material quite workable,as a solid cake!

All 8.2g were purified using a simple acid dissolve and basify.

The material was powderized and then added to 300ml of Water with 100ml Vinegar.

Concentrated sodium carbonate solution was added to produce freebase. The solution was VERY thick and cloudy with goodies.

There was about a 50% loss in alkaloids. Most of this loss was in a thick red\black goo.

Procedure:

1. Took crude extract on a flat plate and chopped it to medium\small bits with a big knife
2. Placed a coffee filter over all the bits so they were all covered
3. Rolled a smooth glass cup\jar over the coffee filter while pressing down very hard. Rolled back and forth.
Note: This breaks up all the hard crude extract pieces into a powder. Repeat as many times as needed.
4. Used a razor to finish chopping and sorting the powder until it was very fine.
5. Added 100ml Vinegar into 300ml Medium-Hot Water
6. Added extract powder into solution
7. Shook violently for 5 minutes.
8. Let settled for a couple hours.
9. Filtered solution through the Homemade Pressure Pump and discarded the dark red goo.
Note: The resulting goo on the filter was very thick, almost like syrupy sediment. Looked very dark red\black
10. Mixed 200ml fresh water with 4 heaping tablespoons of Sodium Carbonate. Settled for 10 minutes.
11. Filtered the 200ml concentrated sodium carbonate solution through a cotton ball filter to remove any excess carbonate.
12. Added concentrated sodium carbonate solution to vinegar\alkaloid solution.
Note: Rapid color change occurred then stabilized.
13. The mixed solution was swirled well and left for 30 minutes to react.
14. The solution was put in the fridge for 2 hours.
15. The solution was filtered through the Pressure Pump onto 5 different coffee filters.
16. The coffee filters were dried in the food dehydrator @ 115F for 45 minutes. Produced 'Harmala Flakes'
17. Powderized flakes using the procedure in steps 1-4. That's it! Put in vial for storage!


Total Yield - 3.7g Semi-Pure Tan Harmaloids - 1.5% Total Yield from 250g Caapi

Really amazing work my friend! 1,5% freebase yield from caapi after clean up is fantastic!

So is there any THH in there or is it all harmine?

I don't know how to tell. I am hoping for a lot of THH, I was seeking this in particular. I hoped that by not doing a salt precipitation Manske style I was able to pull out everything in the Caapi.

I don't see why THH wouldn't behave as other harmalas and crash out of the solution at the right pH. Hopefully the pKa isn't too high but I doubt it would be higher then sodium carbonate can make a solution.

The only way I can think of is to get a friend to run it though a mass spectrometer.

Any ideas?

I don't know how to identify THH. SWIM can easily tell if there's THH in the mix by testing it orally though.

nice work - maybe by doing something like this separation - http://www.dmt-nexus.me/...aspx?g=posts&t=5749 but with a different ph for thh
perhaps thh precips at a lower or higher ph than harmine - with the low amounts of harmaline in caapi this separation process could be repeated until one is fairly happy with the results. Just an idea.

I thouhgh that THH freebase is not a solid but some sort of goo. Or am I wrong ?

no idea - perhaps if thats true then a suitable solvent can be added to the basic solution to pull it after salting the harmine and harmaline out. then that solvent evapped ?

SWIM may be able to run some mass spec analysis. It may or may not be able to happen.

So... this is what I am thinking. Get an analysis on the final material. Test for content & purity.

Additionally, take an acidified caapi extract and split it into 15 parts.

Start with Part 1 and basify to pH 5.0
Take Part 2 and basify to pH 5.5
Take part 3 and basify to pH 6.0

This would continue for the range of pH's from 5.0 - 12.0

The results from all 15 samples would be tested individually and analyzed to determine an accurate pKA prediction for THH.

If the range was determined to be between 6.5-7.5 then another 10 samples will be created.

The first sample would be pH 6.5
The second sample would be pH 6.6
The third sample would be pH 6.7

This would continue until pH of 7.5

These samples would be tested and analyzed to create an accurate pKa estimation for THH.

I know some chemistry graduates who could probably offer tips on experimentally determining a pKa.

Cosmic Lion, it would be uber-cool if SWIY dose the above analysis!

Even though I'm not quite sure how you'll use the mass spec to determine the pKa of THH. Why doesn't SWIY go for standard titration?

don't know bro but if you noticed baron's thh never been in form of freebase. It was either acetate or hydrochloride. That must be for reason. We need to think harder about this. We wasting time to think how to precip. freebase but it could simply be an impossible task.

Hang on. This solvent could be an ethylacetate as suggested in this thread http://www.dmt-nexus.me/...aspx?g=posts&t=7941 Then we could just simply salted thh out of ethylacetate using either acetic or hydrochloric acid, innit. It`s ethylacetate watched in UK ?

Well THH is more expensive to come by so perhaps to make the profit margin better they sell it as salts because salts weigh more. They sell 1g Salts instead of freebase to make up some costs. Harmine and Harmaline are cheap to freebase abundantly.

I agree with retrieving the goods into a solvent.

After the acid extraction basification could take place via Sodium Carbonate until color stabilizes.

The resulting liquid & powder could be mixed with limonene to absorb the alkaloids.

CASW (Citric Acid Saturated Water) could be used to retrieve harmalas as salts.

Or, CASI (Citric Acid Saturated Isopropyl) could be added directly into the limonene to try and precipitate out the harmala salts. Like Jorkest is doing Here.

Any acid could be tried to see if any work better. Fumaric might be a good start.

An interesting experiment would be to run some controls and compare how much freebase is collected using this direct normal method, how much is collected using the salting method and how much is collected if the created salts are freebased by dissolving in water then adding sodium carbonate then collecting precipitants.

It might help isolate if THH really does get lost in the freebasing process.

CosmicLion: I cannot beleive you used 10 Gallons (45 LITRES) of vinegar for a measly 250g caapi. What a waste. but, credit to you, you are obviously a dedicated guy! and good research too.

Do you know where I can find an extraction tek for caapi? If possible, a way to get the THH too. i've just received my 250g and Its gotta be done in a few days time for a very special night of psychedelic music! w00t

Thankyou.

I just want to add that the herbal percolator method has been tested extensively over at the Aya Forums. They have found that ROOM TEMPERATURE water is best to use. It pulls the same amount of alkaloids but leaves behind much of the tanins and plant material that hot water pulls.

And yes, it needs massive amounts of water to be that effective.

by who?

as you can see herel the other harmalas are
'freely souluble in water' and then there isn't any data for THH's solubility.

later it is listed as soluble
in methanol, ethanol, ethyl acetate, dichloromethane and chloroform. Based on that theres a good chance that its soluble
in IPA aswell, since everyone will have that laying around from the BLAB. I am about to test that.

My point is: If I had to guess from what i've read I'd say that THH would be extracted by a manse extraction. I don't see why
not, Chemically if harmine and harmaline are extracted then thh won't be far behind.

Ive got some ideas for a tek, see my thread titled harmala IPA tek. Water extraction is obviously crap...

Lol, 45L of straight Vinegar? Yea right, read the post dude. Every 4 cups of water had a DASH of vinegar in it. I really only put about 1/4 Cup or less of Vinegar per 4 cups of water. I used a little under a gallon of Vinegar... a very cheap substance running like $2.50 a gallon. This is waste by whose standards? I used tap water. An average 10 minute shower uses 40 gallons of water. I used the water equivalent of 3 minute shower. Pretty unsubstantial in the grand scheme of water usage.

It would be a bigger waste, IMO, to not get all the alkaloids out of the vine. Caapi is MUCH more expensive then water or vinegar and it seems ridiculous to only get 1/2 your yield because you argue the semantics of 2 vs 10 gallons of water or are scared of using a single gallon of vinegar.



By general board conjecture. It was theorized, no definite conclusions.

Also, I was aiming for a Full-spectrum extract, regardless of THH. The Jim-Jam of Harmala.

Manske eliminates secondary compounds in Rue so one can only assume there might be SOMETHING in Caapi that gets left behind by doing a Manske, even if it is some secondary alkaloid.

Plus doing a Manske salting is an extra, uneeded, step when extracting Caapi. Why go through the trouble of doing Manske & Filtering when you can just freebase directly out of an acid pull? You would be re-dissolving and purifying either way most likely.