Bufotenine Extraction

[Ethnochemist]

Xylene and Acetone are miscible....how would swiy separate them?

(Well, swim knows how...) SWIM would add acetone to dissolve all the crystals.....then drip in water until the Xylene separates and floats on top...pour it off, and bam! However, if swiy is just pouring off most of the Xylene anyway, it's probably better to just let that small amount evaporate rather than go through evaporating water and acetone as well.

E.C.

 

[prey]

Yes, I think you're right.

 

[69ron]

This may be a dumb question but...

Couldn't SWIY take the freebase crystals that precipitated from xylene, and dissolve them into acetone? The xylene should be liberated from the crystals as they dissolve in acetone, and then they would evaporate away, no?

Of course this could leave some acetone left in SWIY's crystals, but acetone is much less toxic and much more volatile than xylene.

Yes, the xylene will mix with the acetone and some will evaporate away with the acetone. IPA would work better, but take longer. I think neither method will work 100% though, but both are be better than nothing. The problem is, xylene has a high boiling point and doesn’t form azeotropes with a lot of other solvents. So the best way to remove it would be to recrystallize the bufotenine using the MEK:heptane method. That way the xylene stays in the heptane after the MEK is gone. You poor off the heptane, and the crystals left behind should be free of xylene.

 

[Ethnochemist]

Wait hold on, now swim is confused about the MEK:Heptane procedure.

So say...even before the Xylene boil. SWIY has a some brown/amber freebase goo. SWIY would then add MEK:Heptane, mix around a little, pour off the MEK:Heptane, and then evaporate the MEK:Heptane?

And now say there was a Xylene boil, and then one did the procedure swiy outline above, the point of the heptane is to be poured off? How does one know if all the MEK boiled off? And if the point of the heptane is to pour it off, why would one extract the goo with MEK:Heptane in the first place? Why not just MEK?

What is the idea behind the MEK:Heptane procedure?

Thanks,
E.C.

 

[69ron]

Wait hold on, now swim is confused about the MEK:Heptane procedure.

So say...even before the Xylene boil. SWIY has a some brown/amber freebase goo. SWIY would then add MEK:Heptane, mix around a little, pour off the MEK:Heptane, and then evaporate the MEK:Heptane?

Mix 2 parts MEK to 3 parts heptane, by volume. Mix your goo in it thoroughly at room temperature. The freebase bufotenine is soluble in the solvent. The toxins are virtually insoluble in it and sink to the bottom. Let it settle for a minute. Pour off the solvent mix, leaving behind the dark goo at the bottom.

You can then let it evaporate at room temperature to grow some large crystals. What SWIM does instead to speed up the process is to boil it down to 1/2 the volume. At this point most of the MEK has boiled away leaving mostly heptane causing the crystals to form faster. Then let it evaporate at room temperature. Once it’s down to about 1/10 the volume of solvent and you see many large crystals (1-2 cm wide), you can decant the remaining solvent usually. If you think there’s any more in the solvent, after decanting the solvent, put it in a separate container to evaporate completely. You might get another tiny crop of crystals from it.

And now say there was a Xylene boil, and then one did the procedure swiy outline above, the point of the heptane is to be poured off? How does one know if all the MEK boiled off? And if the point of the heptane is to pour it off, why would one extract the goo with MEK:Heptane in the first place? Why not just MEK?

What is the idea behind the MEK:Heptane procedure?

Thanks,
E.C.

If only MEK was used, you’d get a thick goo full of toxins. Bufotenine is very soluble in MEK, but insoluble in heptane. The sticky toxins are also soluble in MEK and insoluble in heptane. However, when 3 parts heptane are added to 2 parks MEK, the bufotenine is soluble in the mix, but the toxins aren’t. It’s about polarity. The toxins are slightly more polar than bufotenine. As you add heptane to the MEK you lower the polarity of the MEK. Once the polarity is lowered to a certain point, the toxins are no longer soluble in it. That point is 3 parts heptane to 2 parts MEK. If we increase the heptane, eventually the bufotenine will no longer be soluble in it either, so we leave it at the minimum amount of heptane needed to make the toxins insoluble in the mix while still keeping the bufotenine soluble in it.

If you boil down the MEK:heptane mix to about 1/2 the volume, most of the MEK will be gone. You can tell by smelling it. MEK smells sweet, heptane smells sort of like gasoline. They smell completely different. Then you let it evaporate to about 1/10 the volume. At that point many crystals should be present and you can pour of the remaining solvent (mostly heptane at this point).

The xylene boil does pretty much the same thing as the MEK:heptane mix. It effectively removes all the toxins. You don’t need to perform both. The MEK:heptane mix is good enough for removing the toxins. The xylene boil is simpler because you only need one solvent and xylene is pretty easy to get for most people. Both are purification procedures.

The MEK:heptane procedure leaves less solvent in the final product because both MEK and heptane evaporate very fast. Also dissolving the final product in acetone and evaporating off the acetone will effectively remove nearly all traces of solvent (because both MEK and heptane will easily evaporate along with the acetone). Acetone is found in the human body and is many times safer than heptane or xylene.

 

[Ethnochemist]

Excellent explanation. Very much appreciated. SWIM can't wait to try this out!.

E.C.

 

[prey]

Seconded, great post.

Another maybe dumb question... from what SWIM understands SWIY is taking advantage of the fact that MEK is much more volatile than heptane while at the same time being a much better solvent than heptane.

Couldn't SWIY use acetone in place of MEK then? Because apparently acetone is a good solvent for freebase bufotenine just like MEK, it is miscible with heptane just like MEK and it is highly volatile like MEK.

Very hard to find MEK in SWIM's area that isn't mixed with mineral spirits and/or methanol.

 

[69ron]

Seconded, great post.

Another maybe dumb question... from what SWIM understands SWIY is taking advantage of the fact that MEK is much more volatile than heptane while at the same time being a much better solvent than heptane.

MEK (evaporation rate=3.7) is actually less volatile than heptane (evaporation rate=4.3). However it boils off faster than heptane because it has a lower boiling point (79.64 C, while heptane boils at 98.43 C). So you can force most of the MEK out of the solution by boiling the solution. All this does is speed up crystal formation. If left to evaporate without boiling off most of the MEK, the heptane will evaporate first. It will take longer for crystals to form, but they will also be larger. But it doesn’t really matter. All that matters really is that the toxins are not soluble in the solvent mix. The toxins prevent bufotenine from crystallizing and also ruin the experience (causing nausea, head tension, etc.).

Acetone has a lower boiling point (56.29 C) than MEK (79.64 C) so it boils off much faster than heptane does. It also has a faster evaporation rate (5.6) than heptane (4.3) and MEK (3.7). It’s probably better to use than MEK. The only reason SWIM didn’t use acetone in his tests was because he was out of acetone and had lots of MEK sitting around.

Couldn't SWIY use acetone in place of MEK then? Because apparently acetone is a good solvent for freebase bufotenine just like MEK, it is miscible with heptane just like MEK and it is highly volatile like MEK.

Very hard to find MEK in SWIM's area that isn't mixed with mineral spirits and/or methanol.

Yes you could substitute acetone for MEK. You could also substitute naphtha or xylene for heptane. But you’d have to work on the exact ratio to use. With MEK:heptane, SWIM tested many different ratios and the correct ratio was found to be 2:3, but as soon as you substitute one solvent for another, you will most likely need to adjust that ratio for that specific solvent mix.

Acetone is more polar (more water soluble) than MEK. So if substituting acetone for MEK, you’re likely going to need to use less acetone. Maybe something like 4:7 of acetone:heptane MIGHT work. Only through testing can the correct ratio be found.

If substituting naphtha or xylene for heptane, you’re going to have to use less MEK because these solvents are more polar than heptane. Again, only through testing can the correct ratio be found.

If acetone and xylene were used as the mix, you could probably use much less total solvent. You would need to find the correct ratio to use. Acetone is more polar than MEK, and xylene is more polar than heptane.


The way to test it is to make 9 different batches of solvent using different ratios. For example:

1 ml : 9 ml of acetone : xylene (or acetone : naphtha)
2 ml : 8 ml of acetone : xylene (or acetone : naphtha)
3 ml : 7 ml of acetone : xylene (or acetone : naphtha)
4 ml : 6 ml of acetone : xylene (or acetone : naphtha)
5 ml : 5 ml of acetone : xylene (or acetone : naphtha)
6 ml : 4 ml of acetone : xylene (or acetone : naphtha)
7 ml : 3 ml of acetone : xylene (or acetone : naphtha)
8 ml : 2 ml of acetone : xylene (or acetone : naphtha)
9 ml : 1 ml of acetone : xylene (or acetone : naphtha)

Put aside 9 batches of your sticky extract. Attempt to dissolve each batch using one of the 9 different solvent mixes. Then evaporate your 9 different solvent mixes. The 1:9 mix will be the stickiest with the most amber toxins and probably won’t crystallize. The 9:1 mix will have a very tiny bit of bufotenine and no toxins and will form a few tiny crystals. You’ll want to find the mix in between those two that has the most crystals and the least amount of amber sticky toxins present. That mix would be the one to use.

 

[Ethnochemist]

SWIM would definitely like to utilize MEK:Naphtha, since Naphtha is much much more available. Unless he finds Heptane at this art store he's going to go to soon.

E.C.

 

[sentient]

69ron

Could SWIM please get a simple step by step method in laymens terms for this extraction from start to finish there is a lot of information here but its kinda scattered. SWIM just wants to be sure of success, and you know so much more than him. SWIM is very much noob, but will be ordering the seeds tonight in hopes to make bufo soon. 100g will be used.

 

[endlessness]

from what I understand the easiest way to extract bufotenine is to first defat the (grounded?) seeds with cold xylene, then mix with sodium carbonate (would BIcarbonate work?), add a little water to make a paste, let dry, put in a resistent container (borosilicate glass or stainless steel), cover with xylene, boil the xylene in hot plate for 5 minutes (very careful, no open flames nearby.. ) , then separate the xylene and let it cool down, and crystals should precipitate. One can reuse the xylene..

Re-dissolving the resulting product in alcohol and letting it evap again in a hot plate will help getting rid of xylene traces

it can be further purified with a mix of MEK/Heptane or there are other possible combinations such as acetone/naphtha, but this needs to tested.

can anybody confirm if what I wrote is right?

 

[Jorkest]

looks good endlessness..its interesting that you mention bicarbonate..because it just might work...how high does the pH go with sodium carbonate..because ive read that bufotenine doesnt like high pH's

 

[Darkbb]

1) Microwave 20g of seeds until the popping dies down.
2) Grind to a fine, flour like consistency.
3) Put in 500mL bottle along with 400mL of VM&P naptha.
4) Close bottle and shake thoroughly (for say, 5 minutes) and let settle.
5) Decant and discard Naptha, retaining seeds.
6) Repeat steps 3-5 once more with fresh naptha.
7) Dry seeds fully, then mix with 50% by volume of either lime or sodium carbonate and sufficient water to make a slurry.
8) Redry seed/base mixture (20 second pulses in the microwave would theoretically work).
9) Regrind to flour like consistency.
10) Put in 500 mL bottle along with 400 mL of acetone.
11) Close bottle and shake thoroughly. Let settle.
12) Decant acetone to evapping dish, being careful not to spill over any seed material and evaporate to dryness.
13) Repeat steps 10-12 once more.
14) Scrape up dry impure bufotenine.

I was wondering does step 7-8 change the bufotenine in any way.

One time I had yopo seeds and all I did was grind up and mix 50% with hydrated lime. Then I proceeded to snort the huge line and I got my first psychedelic effects ever (OEV's) But I tried this again only this time following step 7-8 and letting it dry then proceeded to snort the line and it did nothing. Only I ended up putting about 5-6 hours in between stem 7 and 8.

 

[rellik]

could it be possible that your seeds had a different alk mix w/o or not much bufotenine and more of the more volatile active alks (dmt, etc)?
the heating/microwave may vaporize/destroy the alks that are less boiling point/stable than bufotenine

i remember reading somewhere on the nexus that they have a varying alk mixture but i forget where

 

[Darkbb]

maybe

 

[endlessness]

its possible, theres some crazy genetic variations that result in very different alkaloid content. But AFAIK most yopo contains bufotenine as the major component.

this being said, I in any case have no idea whether microwaves can hurt alkaloids in general.

 

[Jorkest]

from what I understand the easiest way to extract bufotenine is to first defat the (grounded?) seeds with cold xylene, then mix with sodium carbonate (would BIcarbonate work?), add a little water to make a paste, let dry, put in a resistent container (borosilicate glass or stainless steel), cover with xylene, boil the xylene in hot plate for 5 minutes (very careful, no open flames nearby.. ) , then separate the xylene and evap it..

Re-dissolving the resulting product in alcohol and letting it evap again in a hot plate will help getting rid of xylene traces

it can be further purified with a mix of MEK/Heptane or there are other possible combinations such as acetone/naphtha, but this needs to tested.

can anybody confirm if what I wrote is right?

i just noticed something here..if you are doing the xylene boil..you dont need to evap the xylene..just pour it off the ground seeds...and let it cool for a few hours..crystals will drop..and then you can put the xylene back on the seeds and do another boil...at the end of all this after maybe 4-5 xylene boils..you can evap the xylene all the way down to retrieve any bufo that might still be in it

 

[endlessness]

true, just edited

 

[logos2012]

That's way too many steps. There must be a simpler way.

I’m thinking about this possible tech.

Step 1 – Grind and Dry
Coarsely grind 100 grams of fresh seeds. Dry in an oven at 250 F until completely dry.

Step 2 – Defat with Xylene
Boil seeds in 500 ml xylene for 5 minutes. Filter and discard the xylene. Repeat until the xylene comes out clear.

Step 3 – Freebase with Calcium Hydroxide (lime)
Add 1 part calcium hydroxide to 2 parts seeds. Add enough water to form a clay like consistency. Mix for 5 minutes. Dry in an oven at 250 F.

Step 4 – Extract Bufotenine Crystals
Boil seeds in 500 ml of xylene for 5 minutes. Filter out the seeds. Put aside the xylene to cool. Collect freebase bufotenine crystals in a few hours by pouring off the xylene.

SWIM has not tried this yet. He doesn’t have any more seeds. He believes this will work very well. If you defat with xylene, you pull everything out that’s soluble in the xylene. Then you freebase and extract the alkaloids in xylene. Only the bufotenine should dissolve in the boiling xylene. When the xylene cools, bufotenine drops out. It should work quite well. SWIM already ordered more seeds. But it will be several days before he can give this a shot.

Tell me what you think.

This didn't make sense to SWIM. Here it says to defat by boiling the seeds in xylene then discard the xylene. Is the bufotenine not soluble in the boiling xylene because it is not freebase yet?

Later on in this thread it says to defat in cold xylene.

from what I understand the easiest way to extract bufotenine is to first defat the (grounded?) seeds with cold xylene,

Which is correct?

 

[69ron]

That's way too many steps. There must be a simpler way.

I’m thinking about this possible tech.

Step 1 – Grind and Dry
Coarsely grind 100 grams of fresh seeds. Dry in an oven at 250 F until completely dry.

Step 2 – Defat with Xylene
Boil seeds in 500 ml xylene for 5 minutes. Filter and discard the xylene. Repeat until the xylene comes out clear.

Step 3 – Freebase with Calcium Hydroxide (lime)
Add 1 part calcium hydroxide to 2 parts seeds. Add enough water to form a clay like consistency. Mix for 5 minutes. Dry in an oven at 250 F.

Step 4 – Extract Bufotenine Crystals
Boil seeds in 500 ml of xylene for 5 minutes. Filter out the seeds. Put aside the xylene to cool. Collect freebase bufotenine crystals in a few hours by pouring off the xylene.

SWIM has not tried this yet. He doesn’t have any more seeds. He believes this will work very well. If you defat with xylene, you pull everything out that’s soluble in the xylene. Then you freebase and extract the alkaloids in xylene. Only the bufotenine should dissolve in the boiling xylene. When the xylene cools, bufotenine drops out. It should work quite well. SWIM already ordered more seeds. But it will be several days before he can give this a shot.

Tell me what you think.

This didn't make sense to SWIM. Here it says to defat by boiling the seeds in xylene then discard the xylene. Is the bufotenine not soluble in the boiling xylene because it is not freebase yet?

Yes, exactly. The salt form in the seeds is not soluble in boiling xylene, only the freebase form is.

Later on in this thread it says to defat in cold xylene.

from what I understand the easiest way to extract bufotenine is to first defat the (grounded?) seeds with cold xylene,

Which is correct?

Both should work. Defatting with boiling xylene will be more effective but only works if the bufotenine is not in freebase form. If the bufotenine is freebased you can defat with cold xylene, but not boiling xylene.