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Detailed Bufotenine Extraction Pictorial Options
 
blue.magic
#1 Posted : 8/16/2017 11:21:33 PM

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Here is a pictorial of "RebBaron's Yopo Extraction". Take it as a comics for your entertainment.

The vilca seeds has been roasted, deshelled and ground:



Eyeballed the equal volume of sodium carbonate:



Well mixed into watery paste and spread to promote drying:



After drying for few hours, the srapings were ground into a powder with mortar and pestle, further dried in an oven (1 hr at 80 C) and re-ground to make sure I will a fine and dry powder:




Mixed with approx. 30 mL of acetone:



Vacuum filtering through a cotton ball, another 25 mL of acetone mixed in and filtered:



Secondary filtering with glass micro-fiber filter and Celite filter aid. Showing residue on a thin bed of Celite:



The filtrate is now pretty clear, yellowish liquid:




Salting out the alkaloids with citric acid solution (left beaker: 1 gram citric acid in 10 mL acetone). You can see clouding on top:




Alkaloid precipitate, looks like a curdled milk:




Drying, decanting last bits of acetone occassionally:




Now you can see the parts exposed to air turning dark brown:



Drying completed and we have this brown oily sticky mess:



This has been mixed with equal volume of sodium carbonate, litte water added to form a watery paste.
This paste has been set aside for 1 hour, then oven-dried, now clearly showing areas with excess sodium carbonate and the hard caramel bufo candy around:



When scraped, it is surprisingly dry!




Time for more filtering. The stuff has been dissolved in approx. 40 mL of acetone and vacuum filtered (glass micro-fiber, Celite). The filter caught all the insoluble base and some colored residue:



Having clear yellow liquid again, containing our freebased alkaloids.



After evaporating all the acetone, the leftovers turned into hard caramel candy again





And it's dry and quite fragile. When scraped, it bursts into glittering crystalline powder:



The product collected, we have about 65 mg from 5.67 grams of deshelled seed powder, i.e. 1.14% yield:



Beautiful golden-brown crystals. Crystal porn ahead Smile





Testing vaporization. The crystals liquify immediately, just like DMT:



The substance gives off nice smooth vapor which is not unpleasant to smell but slightly irritating when breathed. I took just one very, very small toke.

The substance is extremely potent and nauseating, even at this minuscule amount!

The substance progressively turned dark brown and finally black:




The residue has a DMT-like smell so there is definitely some bufo inside, with unknown amount of 5-MeO-DMT, n-oxides and lots of unknown substances.

I am wondering if there is a purification method not involving fancy chemicals. Desublimating the vapor? Reduction of n-oxide with Zinc? Mini A/B?

Any ideas are welcome. I think I am done with experimenting with bufo as it is too nauseating for me and having a huge, almost toxic body load.
I hope you enjoyed this pictorial even though it is a very simple extraction and nothing new.
 

Trippy glass for trippy people.
 
Ulim
#2 Posted : 8/17/2017 2:01:21 PM

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Looks good.Thumbs up What did you do? Add more water to paste this time?
 
melotikaci
#3 Posted : 8/17/2017 2:28:43 PM

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That's awesome. Crystals look fabulous.

did you get any visuals? or just strong body load?

When I did extraction with my cebil seeds, after making paste and drying, I pulled with ethanol, evaped it and then washed with toluene(bufo is hardly soluble in it). It removed lots of dark, fatty stuff and I got tiny-tiny brownish crystals. I left them on plate to let it dry well but unfortunately, my gf throw all of it away thinking it was some dust Smile
My point is, maybe you can try washing with toluene.
 
ijahdan
#4 Posted : 8/17/2017 5:30:37 PM

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Always nice to have pics of each stage of these teks. Really brings them to life. Thanks for posting them. Like Melotikaci, Id also be interested to know what visual effects you got, as, for myself, the unique visuals are my favourite part of the yopo experience and worth putting up with the nausea and vaso constriction for (sometimes). I hoped a purer extract would lessen the side effects, but sounds like theyre still strong.
 
blue.magic
#5 Posted : 8/17/2017 6:17:59 PM

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melotikaci wrote:
did you get any visuals? or just strong body load?

The body load is several times stronger than the visual effects so it is hard to get any without it being overwhelming.

I had strong visuals on 650 mg of yopo powder (approx. 4 seed kernels, 1:2 lime:cebil ratio by weight) but I felt like having a heart attack. Never more.

Very light visuals and somewhat pleasant body load at 250 mg (a more tolerant friend of mine would go up to 350 mg).

The bufo extract I made is from about 20 seeds but I don't know how much actives has been lost in the process. Still extremely little is needed for feeling the effect, 1-2 mg suffice, though I think it is mostly effect of the toxins, not bufo itself.

The nauseating comeup is so fast it is frightening to me. I will proceed only after purifying the substance more.

Surprisingly, after the bufo wears off, I feel great and like "in the moment", the next day is almost blissful.

Thanks for the toluene wash tip! I have methanol and IPA, not sure if that will work in place of ethanol.
I also found a water droplet when evaporating the acetone so it may have not been dry (hence may have pulled the toxins). I will dry the acetone next time.

I've read at some old thread that reduction of n-oxide with zinc is more effective when bufo is salted with citric acid rather than acetic.

I have to wait until save some money to recycle my solvents and finish other projects, then I get back to bufo and update the thread.
 
blue.magic
#6 Posted : 8/17/2017 6:30:24 PM

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ijahdan wrote:
Id also be interested to know what visual effects you got, as, for myself, the unique visuals are my favourite part of the yopo experience and worth putting up with the nausea and vaso constriction for (sometimes). I hoped a purer extract would lessen the side effects, but sounds like theyre still strong.


Yes, the nausea (though not to the point of vomiting) and vasoconstriction is just too much.

It is possible the seeds are just too old (oxidized) or bad kind. I will see after the purification.
 
endlessness
#7 Posted : 8/17/2017 6:46:46 PM

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Lets get it tested!

Please do 3 or so different extracts to compare different methods or clean up stages, gather 30mg of each and pm me Smile
 
melotikaci
#8 Posted : 8/17/2017 9:26:34 PM

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blue.magic wrote:

Thanks for the toluene wash tip! I have methanol and IPA, not sure if that will work in place of ethanol.

according to this thread bufo is soluble in most of the polar solvents, so IPA and acetone should work well enough.
I only use ethanol because it's very easily obtainable in any nearby pharmacy.

I have 20 gramms of cebil seeds left, will try extraction this weekend if I have time and post the results here or in new thread.
I wonder what effects will the washed one have. I've tried it before toluene wash and had very strong but pleasent body load(5-40mg), no visuals, though.
 
roninsina
#9 Posted : 8/17/2017 11:35:11 PM

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The Bufo threads mention an ethyl acetate cleanup iirc. Also iirc, ethyl acetate is labeled as MEK substitute, in the hardware stores.
"We sit in a circle and suppose,
while the secret sits in the middle and knows." Robert Frost

 
downwardsfromzero
#10 Posted : 8/17/2017 11:55:28 PM

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blue.magic wrote:
I also found a water droplet when evaporating the acetone so it may have not been dry

Did you use anhydrous citric acid? Culinary citric acid is the dihydrate. Anhydrous is sold as a descaler where I am.

Loved the pictorial, btw.


EDIT: of course, I meant monohydrate!
All posts by this user are purely fictitious and provided for entertainment purposes only.
Ora, lege, lege, lege, relege et labora
???
Thinking of evaporating? Save money and the environment! Reuse your solvents!
 
melotikaci
#11 Posted : 8/18/2017 6:37:36 AM

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downwardsfromzero wrote:

Did you use anhydrous citric acid? Culinary citric acid is the dihydrate. Anhydrous is sold as a descaler where I am.

Would it matter? I've used monohydrate with max ion tek and haven't had any problems(or maybe I had but don't know 🤔).
 
Psilosopher?
#12 Posted : 8/18/2017 7:31:02 AM

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blue magic, you are a treasure on this earth.
"Better than a thousand hollow words, is one word that brings peace." - Buddha
 
blue.magic
#13 Posted : 8/18/2017 9:24:43 PM

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melotikaci wrote:
I have 20 gramms of cebil seeds left, will try extraction this weekend if I have time and post the results here or in new thread.


Great! Looking forward to it. It would be great to unlock the magic of bufo.

endlessness wrote:
Lets get it tested!

Please do 3 or so different extracts to compare different methods or clean up stages, gather 30mg of each and pm me Smile


I don't have all the chemicals at hand and other projects going but surely get back to it.

I will try ethanol/IPA/toluene washed extract and maybe the ethyl acetate washed extract (if I manage to make my own, I don't want to buy entire bottle of ethyl acetate just for this purpose...)

Sure I can send vials with samples for testing then Thumbs up

downwardsfromzero wrote:
Did you use anhydrous citric acid? Culinary citric acid is the dihydrate. Anhydrous is sold as a descaler where I am.


Might be the case! The citric acid is indeed the culinary one. Maybe just baking it would remove the water?

I once tried fumaric acid but there was very little precipitate and god knows whether it is really a bufotenine fumarate or something else:



Psilosopher? wrote:
blue magic, you are a treasure on this earth.


Thanks. Although I am not a chemist and cannot contribute much, it's a pleasure to experiment and learn by practice.
 
melotikaci
#14 Posted : 8/19/2017 7:37:14 PM

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I've started experimenting as promised.

took 5 grams of seeds and divided into two parts for different teks. Will post the complete process in new thread.

I've got one question about acidifying:

After I dried the paste and pulled with ethanol, I added ~40mg of vinegar on ~100mg ethanol. It became very cloudy but stayed that way, nothing precipitated. Then added soda carb, still nothing. measured ph, it's around 8. filtered the liquid with coffee filter to remove excessive soda carb. and left that way.

Any ideas how can I proceed with it?
 
blue.magic
#15 Posted : 8/27/2017 5:17:59 PM

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melotikaci wrote:
After I dried the paste and pulled with ethanol, I added ~40mg of vinegar on ~100mg ethanol. It became very cloudy but stayed that way, nothing precipitated. Then added soda carb, still nothing. measured ph, it's around 8. filtered the liquid with coffee filter to remove excessive soda carb. and left that way.


Are you sure the acetate salt will crash out of ethanol and that the ethanol is anhydrous? I also haven't found any data on the bufotenine acetate solubility in ethanol.

Do you think acetic acid can be substiued for citric? My citric acid has water in it but I have 99.8% glacial acetic acid which would be much easier to use.

I will get fresh ethyl acetate tommorow so I will try new extraction routes incl. washing. I hope the extract will be pure enough enabling bufo to crystallize out of it. I've read water has to be avoided at all costs or bufo won't precipitate.
 
blue.magic
#16 Posted : 8/28/2017 11:14:44 PM

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Okay here is the extraction protocol to obtain A. Peregrina sample extracts for lab testing:

#1 original extract

Already made.

#2 fixed original extraction

Same as the above, only this time the citric acid is anhydrous (baked at 90 C for over 2 hours).

#3 IPA wash and de-fatting

The dried paste will be pulled with IPA; dried; de-fatted with n-heptane or naphtha; dried; then standard acetone extraction will proceed.

#4 Ethyl acetate wash

The extract #3 will be dissolved in dry ethyl acetate, some will be evaporated and we hope some bufo will crystallize out of it. If not, it will be left to evaporate completely.

#5 n-oxide reduction

I may try n-oxide reduction and re-crystallization from ethyl acetate. This will at least rule out presence of bufotenine n-oxide.

Any suggestions are welcome.
 
melotikaci
#17 Posted : 8/29/2017 4:02:30 PM

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blue.magic wrote:

Are you sure the acetate salt will crash out of ethanol and that the ethanol is anhydrous? I also haven't found any data on the bufotenine acetate solubility in ethanol.

Do you think acetic acid can be substiued for citric? My citric acid has water in it but I have 99.8% glacial acetic acid which would be much easier to use.

I will get fresh ethyl acetate tommorow so I will try new extraction routes incl. washing. I hope the extract will be pure enough enabling bufo to crystallize out of it. I've read water has to be avoided at all costs or bufo won't precipitate.

Ethanol was 96% so I guess that was the reason it didn't precipitate.
After evaping ethanol I pulled again to separate it from excessive soda carb that dissolved in solvent.(had to do it ~2 times).

After last evaporation I got golden-brownish crystals, much like the one you got but way more(266mg from ~2grams of toasted/deshelled seeds, that's obviously too much, I'm out of NPSs so will do wash when I resupply).

I don't see a problem using acetic acid instead of citric. Guess acetic would be even better.

Looking forward to your test results.
 
blue.magic
#18 Posted : 9/4/2017 2:41:47 PM

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Okay here is the summary of the last few days of extraction works. I will focus on just the second extraction.

The freebased Yopo powder have pulled with IPA and de-fatted with lots of heptane (five washes were necessary) - now it looks quite dry with bits of "soft caramel" consistency. These refused to dissolve in heptane:



This powder has been subjected to standard A/B (acetone, citric acid) procedure. The citrate salts crashed out immediately:



The citrate salts drying, turning into caramel mess again:



It has been freebased in distilled water, dried, pulled with acetone and dried again to yield the brown hard-candy that turns into crystalline powder when scraped:



Finally, this has beed dissolved in ethyl acetate and filtered.
The ethyl acetate solution contained off-white clouds (bufotenine?) with some insolubles on bottom. I've used additional warm ethyl acetate to dissolve the clouds and filtered the solution to get rid of the impurities:



The amber-colored filtrate should contain bufotenine, that should be able to crystallize or precipitate from it:



Unfortunately, nothing happened after 2 days in fridge, except for very small brown circles on the bottom of the glass.

I transferred the liquid to a Pyrex dish, evaporated a bit (more dark-brown circles appeared) and placed it in the freezer. Will see tommorow if something will finally appear.

I am a bit skeptical anything will come out of this.

I dug deeper in the forum and found 69ron proposed dual solvent crystallization (using MEK and heptane in 2:3 ratio, boiling off MEK leaving bufotenine to crystallize on bottom while the heptane catches all the impurities). Then 69ron proposed even simpler extraction using boiling xylene.

I have both MEK and heptane so maybe the dual solvent crystallization would be a way to go if bufotenine refuse to crystallize out of ethyl acetate.

I don't want to work with xylene (especially boiling it!) nor with fomaldehyde (part of the only working proven tek known, developed by J. Ott).
 
blue.magic
#19 Posted : 9/4/2017 2:54:23 PM

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So further ideas:

- always deshell the seeds! it seems to provide much purer product even with simple "dirty" extraction
- maybe use lime instead of sodium carbonate; what it the current state of the calcium bufotenate myth?
- do alcohol extraction first
- do de-fatting of the freebase extract with polar solvent, in which butoenine freebase is insoluble (naphtha, heptane, toluene, xylene)

- do A/B extraction with DCM instead of acetone, pour in xylene (would toluene work as well?) heat, pull xylene layer and slowly cool to yield purer bufo crystals

OR

- do A/B extraction with MEK, pour in heptane, boil off MEK to yield slighly dirty bufo crystals
 
endlessness
#20 Posted : 9/4/2017 4:18:31 PM

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Oh god please do NOT boil xylene, I've done that once, it did NOT work well (cant remember why) but I can certainly remember it smelled HORRIBLE, and I did it wearing a mask, outdoors.. LOL

Thanks for sharing all these experiments, btw, and yeah lets talk once samples are gathered so we can test it all Smile
 
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