195g of Caapi Shredded were split into two batches of 97.5g
I wanted to compare the THP method with powdered and shredded vine, to see if powdering was really necessary, since the wiki was inconclusive about it.
So I powdered batch #2 and left batch #1 as is, then constructed two identical Herbal Percolators.



Then I began pouring water+vinegar through the percolators. I boiled the water, added vinegar and waited till it was cool enough to funnel through without melting the plastic bottle. I used the following ratios of H2O:5% acetic acid 1.7l:0.1l.

Here you see the THP for the shredded vine and the color of the tea that came out.


And here is the THP for the powdered vine. The tea was notably darker here.


All in all I used 9l of liquid on each batch. Then the fun part began of reducing 9l of each batch to a workable amount, which is something between 400-700ml for me. Though the liquid was pretty light for the shredded version it turned very dark upon reduction:


Finally after many many hours I filtered the liquids into separate jars and basified using Sod. Carbonate.

when adding the Sod. Carbonate you get some foam on top from the reaction with the acetic acid

After what I estimated to be enough sod. carb. I decanted. For both batches I performed the test on the decanted liquid to see if there was anything left in there by adding more sod. Carbonate. For batch #2 I got more clouding and a very white precipitate. Since this looked different from the other precipitates I decided to treat it separately.
(sorry I forgot to take a picture of it at this stage :/ )

After washing several times, I let it dry. The next day I redissolved both batches in acetic acid and filtered out some black insolubles. Basified again. washed about 7 times until the water was clear. Each time I decanted the liquid I decanted through a coffee-filter to catch the floating goodies too.
I did not re-A/B the white stuff since it appeared to be ... white. I just left it the way it was.


Finally I let the cleaned product evap in a baking dish in my oven on low with the fan on.
These are the results:
Shredded


0.9g


Powdered


1.8g


plus the white stuff 0.325g


makes a total of 2.1g equalling or even surpassing my 5*45min boiling experiment with the same vine.

To summarise:

#1
shredded, 9l warm H20+acid: 0.9g

#2
powdered, 9l warm H20+acid: 2.1g

I think the result speaks for itself.

Much love
Enoon

Edit: As was pointed out below my extract is very dark so I decided to do some purification steps on all of my extracted alks. The purified results are the following:

From just boiling caapi 5*45min yield was: ~ 1.1-1.3%
From the THP with shredded I got a yield of ~ 0.43%
From the THP with powdered I got a yield of ~ 0.8%
From the cold extract after 3*3days yield is ~ 0.8%
From the cold extract pulls 4 & 5 yielded... ~ 0.4% so total of 1.2%

Awesome, very appreciated!! More knowledge for the community

Great findings Enoon!

Thank you for exploring this for us all. I will make sure my vine is powdered when I extract it.


Kind regards,

The Traveler

Great work enoon!

Let us know how the final result was with your bioasssay

Thanks for doing this experiment!

It’s possible that the results are not as clear-cut as they seem to be. Caapi extractions produce lots of insoluble sediment. This sediment can be removed by acidifying the crude extract, allowing sediment to settle, discarding sediment, and then basifying again.

Your product looks to be heavily contaminated, so the final weights aren’t telling the whole story. For example, we might expect there to be more insoluble sediment from a powdered product than from a shredded product, so much of the weight difference might be impurities.

(The attached photo shows the result of one of my caapi extractions, which included a step that removes insoluble impurities.)

edit: Whoops! I guess I should pay closer attention to what I read!

I see you mention removing insoluble impurities by acidifying and re-basifying. But how do you explain the dark color of your product? My extraction results have always been beige – very pale, almost white.

(Also, the product you say is white looks like cinnamon to me. Is it the photo or ??)

@ Dagger, it was def. not 100°C since the bottle couldn't have handled that. Unfortunately I did not measure due to lack of a thermometer.

@ gibran2, I wish I knew why my extracts are so dark. Interestingly the powdered one actually seemed lighter before acidifying and basifying for the second time. There was a lot of black stuff that was filtered out for both extracts. I used two coffee filters inside each other to filter out these particles and I filtered both extracts twice through their filters respectively.
The *white* stuff does indeed look like your picture, it's very light colored, the photo just makes it look darker.
The other stuff however is fairly dark and reddish -like cinnamon - even though the water that came out of it was clear with maybe only a hint of a red tint. I treated both extracts the same so it would surprise me if one had a lot more contamination than the other, however I wouldn't rule it out. Perhaps my filters aren't doing their job right...
I'd be interested to hear if anyone else was having similar colored results, or if someone could point out to me what I'm doing wrong here.


cheers
Enoon

I never filter – take a look at this thread to see my method. Maybe when filtering your acidified solution, some solids passed through the filter? At that stage of purification, you should have a crystal-clear yellow solution.

thanks gibran2,
my color takes a long time to change from orange to yellow to clear. I've found I need to do a second A/B step and that seems to yield almost white stuff. However I lose a lot of weight this way.

May I ask how long you usually wait for the harmalas to settle? it seems it takes hours, so instead of waiting I just use coffee filters to catch the rest of the floating harmalas once the majority of them has settled. Not sure if I'm losing a lot this way.

It sounds like your results are very different from mine. Maybe it’s the variety of caapi? I’ve used black and yellow, and black produces the cleanest results.

With black caapi (as I used in my pictorial), most of the alkaloids settle within 5 minutes or so and the solution is nearly clear within another 20 minutes. I collect and save the liquid I siphon and allow it to settle overnight – in the morning it is crystal clear. (Yellow caapi seems to produce a finer precipitate which takes a bit longer to settle.)

Anyhow, it’s hard to say what’s going on, but two A/B steps to get a clean product? That sounds strange. The alkaloids are actually very clean after the first basification. In fact, if one doesn’t mind the solid impurities, the acidification step wouldn’t even be necessary.

yes it took two to three A/B steps to get white alks, the impurities I filtered out were black the first time, the second time they were dark red and the third time also dark red, but less of them. I used white vine from MHUK, I think. Could be that it makes a big difference. I've tried using distilled water and tap water but it made no difference.

Three A/B cycles?

Something about your technique doesn’t sound right – if you remove all insoluble impurities during the first acidification cycle (after the first basification), then how can you get more insoluble impurities later? That’s strange.

Regardless of method, you should have a crystal-clear yellow solution after the acidification step. No cloudiness at all.

Yes it's quite strange... I redissolve in warm acidic water and then I get a sediment. It's possible that I didn't wait long enough for the sediment to crash out before filtering/transfering the liquid. however the liquid was clear but orange iirc. Still get cinnamon colored alks. Repeat, more sediment... I don't know how it manages to stay in solution sometimes, and other times it falls out... it's a mystery and I think the harmalas are messing with me
evil little chemicals.

Anyway I lost about 45% of my weight after several purification steps and got a nice white product. Final yield from the THP part of the powdered vine was 1.18g so approx. 1.2% yield, while the shredded one only yielded about .5%

I extracted the rest of the almost 200g vine together by boiling and yielded another 902mg of white extract. All in all that makes 2.53g out of 200g vine, so again a yield of 1.27%. This being white vine, does this seem realistic, or is it abysmally low?

Enoon,

Can you try another acidification again and then base it with LYE? Just to see if that makes any difference in cleaning.


Kind regards,

The Traveler

I’m not sure if it will make a difference, but dissolve the alkaloids in vinegar and then dilute with water rather than dissolve in already diluted acid. Maybe they’re not dissolving completely.

I’ve done all of my basifications using NaOH, so maybe sodium carbonate doesn’t work as well? Try as The Traveler suggested.

I recently completed an extraction of yellow caapi and got a yield of just under 1%, yet my best black caapi extraction yielded 3.4% - both extractions yielding pale beige alkaloids. Alkaloid content can vary quite a bit.

Ok I finished up another extraction (the cold soak) today and used lye instead of sod. carbonate, as per Travelers suggestion. The precipitates were clean and much finer than with the sod. carb. No excessive cleaning was necessary with this method.

It seems using sod. carbonate you get a strange coagulate that probably traps quite a bit of coloring in it, which is why I needed so many re-acidification steps. With lye it worked really fast, however the alks took much longer to settle.

I updated my primary post with the summary of the total yield I got from all three methods if anyone is interested. The yields have an error of say ± 0.2, estimated. So total yield for method __SOMETHING__ is x±0.2 % where x can be found in the original post above...

Excellent work I don't know how I passed this thread up!

i was wondering if anyone else has had trouble filtering finely powdered caapi? i have so any suggestions are welcome...

funnel + cotton ball
strainer + paper towel(s)

hope this helps.


also someone mentioned lime (CaOH) worked well for precipitating harmalas, has anyone tested this?

the cotton ball funnel was what i was doing, i have turned to cotton linen tied to a stick hanging over a strainer in a pot...it seem to be working wonders...highly recommended if anyone else has straining issues i am also curious if anyone knows about crashing harmalas with CaOH

Yes, I found a new method that works great.

I use a water sediment filter and it filters almost everything in a matter of seconds.

All you need is a water pump... or if you already have a water pump...

Connect lots and lots of stacked cotton wool in a funnel to the water pump to suck the water through the cotton.

See my threead here:

https://www.dmt-nexus.me...aspx?g=posts&t=67223