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Research 2020 Bufotenine Extraction TEK + Analytical Data

Research done by (or for) the DMT-Nexus community
Migrated topic.
Thanks Woolmer! I did not see Trip's points on citrate and fumarate goos, not crystalline but still sounds reasonable to get some separation done.

Will try the shortcut way of Loveall with the boiling acetone step.
 
It works! A no-brainer tek. Followed the proportions in the Loveall tek.

- toast seeds (10 g) and grind
- add sodium carbonate and spray until doughy, incubate for 1-2 hr
- oven dry (material turns dark)
- mix with acetone, warmed until boiling acetone for 10 min with some mixing
- decant and re-pull with acetone (total 80 mL)
- add-in dry magnesium sulfate to collected acetone fractions (about 10 g) with occasional mix for 2 hr and rest to decant
- filter yellow liquid
- Add MASA or FASA, clouds form
- room temperature incubate and watch slightly brown crystals grow!

Working from seeds and there is no need for defatting? Unbelievable! This easy with minimal amount of reagents? Dying to see analytical data. Once yield is finished will post images.
 
From 10 g into 100 mL boiling acetone to half FASAd and the other half MASAd, then the small crystalline precipitates were collected and acetone washed-decanted at room temp-many times until acetone was no longer turning yellow. The final dry yield of the tan-light brown materials were 56 mg fumarates and 80 mg malates. That`s 136 mg out of 10000 mg, 1.36%. Great yield for a pilot experiment. There was probably more 15 or so that was lost due to minor accidents and voluntary tasting. Smell is wonderfully DMTish, but the taste is not quite as bitter. Active, for sure.

Few big leaf-like crystals would easily form on a conical bottom tube, but on a flat bottom tube it formed more numerous but smaller grains (not powder). All in room temperature. The left over acetone was left on the freezer with maybe some insignificant powdery stuff that dropped.

Images are the MASA material only and them both collected into tubes, fumarate on the left, malate on the right... a bit more flakey and subtle darker tinge on the malate.

Thank you, kind participants of this thread!
 

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A third trial using 10 g seeds and about 150 mL of acetone yielded 170 mg malate material. An improvement, likely due to the increase in solvent and so there may be more than 1.7% in them. We also squeezed the seeds mush while sodium carbonate wet, this also might have helped.

A interesting observation is that the magnesium sulfate loaded acetone drying step, or rather a loaded acetone that is as dry as possible, seems to be essential for clean yields. In fact, the mg sulfate salts turns dark brown and the loaded acetone turns light yellow. Without this step, while MASAing clouds do form but there is little clearance and precipitation.
 
I ran a TLC plate for the whitest sample I had from this extraction. The bufotenine lanes are marked with the arrows... The other are harmalas (HCl and freebase). The bufo seems to be of decent purity? Only 1 clear spot that I can see. I should have ran the other darker samples alongside but for some reason I didn't.🤨
 

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I'd like to report that bufo benzoate has poor solubility in water. It took ~ 60 ml of hot water (~80 °C) to dissolve 500 mg of bufo benzoate. This is significant because it shows that the acetone does not have to be so dry upon the addition of benzoic acid, as it will not lead to significant yield loss even if there is some water present. This is another factor to simplify the tek further.

To the solution of bufo benzoate I added a conc. solution of sodium carbonate in water. No precipitate formed but the colour changed from light yellow to dark purple. I evaporated this using a microwave until there was < 10 ml left. A purple precipitate has formed and the solution is currently in the fridge. Will update with pics later.
 
I'd like to report that bufo benzoate has poor solubility in water. It took ~ 60 ml of hot water (~80 °C) to dissolve 500 mg of bufo benzoate. This is significant because it shows that the acetone does not have to be so dry upon the addition of benzoic acid, as it will not lead to significant yield loss even if there is some water present. This is another factor to simplify the tek further.

To the solution of bufo benzoate I added a conc. solution of sodium carbonate in water. No precipitate formed but the colour changed from light yellow to dark purple. I evaporated this using a microwave until there was < 10 ml left. A purple precipitate has formed and the solution is currently in the fridge. Will update with pics later.
Ages ago when I was originally experimenting I too got purple crystals. But I can't remember the process I used, and if it was via bezonic acid, I likely reported it on here.
Do either of you recall the amount and type of incident light when the purple colour formed? I'm wondering about photosensitivity, and whether purity can be improved by using dim red light during the base phase.
 
Found it on pg 2 Tranfrom. I would have just been usual day light from the kitchen window. I apparently did an EA harmala approach tek to the bufo. Sodium carb base paste with little water, EA pulls then crashed it out with citric acid before rebasing with sodium carb. Water went purple and black/ purple crystals crashed out.
 
Do either of you recall the amount and type of incident light when the purple colour formed? I'm wondering about photosensitivity, and whether purity can be improved by using dim red light during the base phase.
I did it during the night in my kitchen which has a "cool white" light colour (4000k?). Not sure though whether colour indicates purity in this case?
 
I did it during the night in my kitchen which has a "cool white" light colour (4000k?). Not sure though whether colour indicates purity in this case?
This would contain a higher proportion of blue (higher energy) light than a warm white bulb. I'd be intrigued to know how a bufotenin extraction turns out when performed under red light.

But indeed, the purple material is likely to be present at a low concentration, so the effect on purity is probably correspondingly negligible.
 
A couple of questions then...

Water in the loaded acetone, yes or no?

Defatting before acetone pull, yes or no? If yes for last one, which nonpolar to use without pulling freebase bufotenine?

My latest attempt with 10 g is yielding more than before (3%), this time it was a very dry loaded acetone that I added a droplet of water and put it in the freezer. Got larger coagulates/precipitants instead of powder (excluding the fats that make white precipitates, but dissolve back at room temp). Next time I will split into tubes and try different things before adding acid like pre-drying, with and without amounts of water and so on.
 
I think a defat is not necessary. The sample I ran on TLC which showed only 1 spot was without any defat.

What are you salting with? With BA I think having dry acetone is perhaps not that important since it has a poor solubility in water. Also, I don't know at what rate acetone absorbs water, but my pulls stood for several hours after BA addition so surely the acetone would absorb some water in this time.

This might vary with other salts though as we don't know their solubility in water.
 
I am salting with malic acid as masa. Seems to work better than fumaric.

Wouldn't fat prevent precipitation? It seems to have a lot of it.
 
Wouldn't fat prevent precipitation? It seems to have a lot of it.
I guess it depends how much fat is being pulled and the solubility of bufo malate in the fat.

Have you tried seeing how much bufo malate crashes out without putting it in the freezer. This way you might not have problems with the fats.

I never placed my solution in the freezer. I think most crashed out at room temperature as placing it in the fridge did not seem to make more crash out.
 
Have you tried seeing how much bufo malate crashes out without putting it in the freezer. This way you might not have problems with the fats.

I never placed my solution in the freezer. I think most crashed out at room temperature as placing it in the fridge did not seem to make more crash out.
Actually have tried this. Indeed it easily drops at room temperature like loose small flakes and powdery light brown stuff, but in the freezer it slowly drops darker and denser brown crystals. Room temp is certainly faster, but I wash the precipitant with clean acetone and if it is too powdery it likely loses some in clean acetone.

Haven't tested the darker material yet. Hopefully all of this replicates the two samples you ran in the tlc plates and both are equally active and safe.

Another question... Light or dark brown it doesn't seem soluble in ethyl acetate. Which one would be best for cleanup, acetone or EA?
 
Another question... Light or dark brown it doesn't seem soluble in ethyl acetate. Which one would be best for cleanup, acetone or EA?
Not sure. Have you tried dissolving it in hot EA or acetone? Maybe you can re-x this way. I guess it's just something that needs testing.

Otherwise, you could also try washing with cold EA or acetone, and compare yields before vs after.
 
Tried washing the dark stuff in boiling acetone or EA. It doesn't lose the color. It has a stronger taste and smell (nutty, like the seeds) compared to the tan stuff. My suspicion is that it is a dark colored pigment in the seed hulls, maybe taking that out before cooking and grinding. Overall similar effects to the tan stuff but no systematic evaluation.

It was not a lot of the yield, around 3% total and the dark stuff only 0.4% or so. I low MASAd the loaded acetone and put in the freezer, let it crystallize (this came as the dark - yellowed stuff), then the still loaded acetone was decanted to another Glass and then heavy MASAd at room temp and refrigerator, which gave me light tan small crystals that were hot acetone washed until acetone came out transparent (2 washes). This was dried and is more like a light tan powder than whatever I got before which were mainly crystals and flakes dark yellow or yellow-brown. It tastes a little bit bitter and very nutty, no smell. No taste of malic acid whatsoever (nnDMT from masa or fasa do taste like malic and fumaric acid).

Now, with the light tan stuff I have tried insuflatting up to 5 mg (many times in a single day, thankfully it does not burn like NNDMT) with and without harmine freebase. Sublingual up to 20 mg with and without harmine freebase. Intramuscular up to 20 mg. Will eventually try vaping and evaping. Effects vary in each type of administration. Lasts a minimum of 1 hour and a half, with a long tail. Somewhat electric feel. Colors and textures intensify beautifully, the visual acuity feels like hallucinations. A distinct spacial sense with open and closed eyes. Oevs and cevs have a pulse to them and are more like a glimmer or static instead of well defined shapes and colors. Overall not very visual. Music also wasn't very different than normal state. Not emotionally engaging, very neutral. You can stop tripping and go do something and come back and it's still thereI, very persistent and non-debilitating. IM is a different beast, and you get clear visuals and hallucinations at peak effects plus everything else I mentioned. Ended up being very different from NNDMT. I was considering the sayings of 2-4x stronger than DMT but it doesn't make sense to me now. I would gauge that 30 mg IM gives you the full effects for either but bufo lasts 2-3x more.

All felt very safe and healthy. No vasoconstriction. Maybe a little bit of nausea when insufflating and oral-sublingual.
 
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