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Psilocybin Extraction: how to really do?

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martiN211

Martin211
Psilocybin Extraction: how to really do?

Hi everyone :)
i'm italian so i ask sorry if my english is not so good. but i'm shure we can understand each other.
So, i want to do a psilocybin extraction and see a nice crystal ;) i look in the web and i found something, but nothing that really explain how to do.
1) i see the PF fanatics tek that use only the alcohol. but everyone say that the "white powder" that you see after the freezer precipitation is not the magic, but a mix of sugar. Also on the website truffelmagic, they explain how to do an alcool axtraction, but they add a cleaning phase whit naphtha and acetone… but is the same.
2) so i look the FBI report on the fanaticus website. if i understand good,
they put the mushrooms in the methanol for 24 h.
after they filter the liquid and they reduce it like 1/10.
after they add sulfuric acid.
This solution was washed twice with chloroform.
The samples were made basic with sodium bicarbonate and the psychoactive drugs were extracted twice with chloroform.
The chloroform was evaporated and the sample was reconstituted with methanol.
3) On rhodium i find this tek, but i don't understand it so good:

A representative sample of 2 to 10g of dried mushrooms is ground to a fine powder by mortar and pestle. The powder is mixed with 100 mL of dilute acetic acid in a 250-mL beaker. The pH is readjusted to pH 4 with glacial acetic acid. After standing 1 h, the beaker is placed in a boiling water bath for 8 to 10 min or until the internal temperature of the acid mixture reaches 70°C. The beaker is removed and cooled to room temperature under running water. The acid mixture is separated from the mushroom powder by suction filtration using glass wool. The filtrate is brought to pH 8 with concentrated ammonium hydroxide and quickly extracted with two 50-mL portions of diethyl ether. Gentle mixing instead of shaking should be used to prevent an emulsion. The ether is dried over sodium sulfate, filtered, and evaporated under nitrogen with no applied heat.
Crude psilocin will appear as a greenish residue. Recrystallization from chloroform/heptane (1:3) yields white crystals. The resulting powder can then be submitted to infrared and mass spectral analyses.

So, now i don't know where from start.
I was thinking: isn't it better to make a tea with mushrooms, so that psilocybin goes into the water, and then extract it with methylene or some how??
So, in the end… If someone know how to do a good extraction… please let me know =)
Thank you all ;)
 
The only kind of extraction I’ve heard about, I read in my only shroom cultivation book I have. It’s an alcohol extraction that results in a tincture, not crystals. Dosnt sound like what your looking for though.
 
So both TEKs seem not wrong, so why not just trying them?

The thing about Psilo extraction is I think that it seems hard to get a really pure extract and its likely to be not that stable ...

I thought it would just be the best to leave it in the mushrooms ... but of course thats no good answer if someone WANTS to extract them.

But those TEKs dont seem wrong - any reason why you dont wanna use them?

The first one uses Methanol, thats not extremely healthy and the second one uses somehow more kitchen friendly chemicals, just pay attention with the ether - you can google about ether safety easily. Chloroform is also not really healthy, but just for recrystallization it should be better than using Methanol from the other TEK.
 
Yes amico 10min in hot water, with swirling and squeezing the shrooms with a spoon, will extract all the actives into the tea =) the PF crystals of gods tek turned out to be sort of bogus. Maybe he thought it made sense and was honest, maybe not and it was just using hype as a tool for comercialization, for PF was selling stuff and making a living off psyches.
 
Brennendes Wasser said:
So both TEKs seem not wrong, so why not just trying them?

The thing about Psilo extraction is I think that it seems hard to get a really pure extract and its likely to be not that stable ...

I thought it would just be the best to leave it in the mushrooms ... but of course thats no good answer if someone WANTS to extract them.

But those TEKs dont seem wrong - any reason why you dont wanna use them?

The first one uses Methanol, thats not extremely healthy and the second one uses somehow more kitchen friendly chemicals, just pay attention with the ether - you can google about ether safety easily. Chloroform is also not really healthy, but just for recrystallization it should be better than using Methanol from the other TEK.
Click to expand...


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i think that i need to try and see, how you say. now that you tell me that the two teks are good, I'm a little more confident. So i think to start whit the first one and see.
And yea, i want to do a extraction because i eat to much mushrooms and now i feel the "bad" fisic effect so much. And also because i want to try to do a magic candybear whit extraction of mushrooms inside;)
so for now thank you ;)
 
Hi. We've been at this for a while and found that psiloc(yb)in extractions are hard. We have a collaborative thread were we were able to crash psilocin fumarate from xylene. However the process is cumbersome and yields are low, but anyone interested in this path could continue the work (I'm not doing this at the moment).

For anyone wanting to work on this, I reccomend exploring the following path:

- Buy Na+ based cation resin (used for water softening commercially) and setup cheap column filled with resin.
- Get some tryptophan and practice getting it on the column and off the column. You can use reagents to track if the molecule is on or off the column. To get it on the column, use an acidic water solution. To get it off the column increase the ionic strength (250mM) and add some ethanol (20%) but keep it acidic. Working at pH4.
- A good salt to increase the ionic strenght is ammonium acetate since it is volatile.
- If you learn how to get tryptophan on and off the column, get a small desktop freezer, a vacuum pump, and build yourself a freeze dry setup. Recover the tryptophan with it.
- With mushrooms work in the dark and quickly to minimize air exposure under mildly acidic conditions (pH4).
- Do a water extract at pH4 for 1h at 70C, everything should be psilocin in water after that.
- Use the column to isolate psilocin, the techniques developed for tryptophan will help.
- Freeze and dry the isolate coming off the column. The resulting stuff (psilocin acetate) should be active/pure. To increase lifetime and powderiness this mixing HPBCD before freezing may help.

This is currently what I'm working on. There is a thread with details on the site. Anyone that wants to join this effort is very welcome.
 
Loveall said:
Hi. We've been at this for a while and found that psiloc(yb)in extractions are hard. We have a collaborative thread were we were able to crash psilocin fumarate from xylene. However the process is cumbersome and yields are low, but anyone interested in this path could continue the work (I'm not doing this at the moment).

For anyone wanting to work on this, I reccomend exploring the following path:

- Buy Na+ based cation resin (used for water softening commercially) and setup cheap column filled with resin.
- Get some tryptophan and practice getting it on the column and off the column. You can use reagents to track if the molecule is on or off the column. To get it on the column, use an acidic water solution. To get it off the column increase the ionic strength (250mM) and add some ethanol (20%) but keep it acidic. Working at pH4.
- A good salt to increase the ionic strenght is ammonium acetate since it is volatile.
- If you learn how to get tryptophan on and off the column, get a small desktop freezer, a vacuum pump, and build yourself a freeze dry setup. Recover the tryptophan with it.
- With mushrooms work in the dark and quickly to minimize air exposure under mildly acidic conditions (pH4).
- Do a water extract at pH4 for 1h at 70C, everything should be psilocin in water after that.
- Use the column to isolate psilocin, the techniques developed for tryptophan will help.
- Freeze and dry the isolate coming off the column. The resulting stuff (psilocin acetate) should be active/pure. To increase lifetime and powderiness this mixing HPBCD before freezing may help.

This is currently what I'm working on. There is a thread with details on the site. Anyone that wants to join this effort is very welcome.
Click to expand...

This is interesting. I am curious though, why do you not follow the same procedure Hofmann originally used to isolate psilocybin? Or some variation of it? I know you are aware of it, it's been mentioned in the threads you discuss the extraction of psilocybin, yet nobody seems to have actually done this, instead opting to reinvent the wheel.

Or is that what you are doing, and using this on the methanol extract that results rather than the chromatography column?
 
Yeah, the Hoffman method was looked at. Several solvents not easy to get where used and also halogens where precipitated with chemicals. Was a long process too.

Since Hoffman, a cation resin exchange method has been published which looks very simple (see papers in this post). Now trying to recreate that.

The cation resin method published does use methanol in dilute HCl (50mM) to extract the mushrooms which is then loaded onto the resin. That is a very good option. I tried this but something went wrong, need to troubleshoot. When I use acidic vitamin C water only it seems to work better in my particular situation. Instead of a UV sensor, to detect psilocin we are using a vanillin/HCl/ethanol reagent (other reagents could be used).
 
The solvents aren't actually difficult to obtain at all. Expensive, but not difficult. I guess I might just know the right people.

So, you say halogens come along with the psilocybin, I'd assume this comes from the chloroform? I remember reading about this, but no explanation was given. I can't imagine they make it through the column though? And, what exactly is the concern here? I guess it's probably not healthy.

I feel as though I read benzyme saying supercritical co2/butane extraction would make for a suitable defeat step which should replace the need for halogenated solvents. Or did this end up not being the case? If so, co2 is cheap. It wouldn't be much concern if several pounds were needed for a small batch.

I know of another, far more nefarious instance where ion exchange resin is used for extraction. Elution is accomplished by reversing the flow and running brine through.

Also, in this case there is a substantial loss of product over the first few runs(~50%) that stays bound. This could be something to consider in testing the ion exchange- it will likely need to be repeated with the same resin to see positive results

I'm gonna read through that thread now. Thanks. I'm very interested in this subject, I wanna get as much info as possible, you know stand on the shoulders of giants and all
 
Right, the Hoffman method solvents can be gotten and such, it's just what it seems that the cation exchange method published in 2010 could be more straight forward.

There are fancy cation resins now that are durable, reusable, and high quality and very cheap.

In essence that's why we are trying them out. Would love more hats in the ring so we can figure it out together.

It doesn't stop as psiloc(yb)in. Molecules like Harmalol, and also the classics may be available without having to use a hydrocarbon solvent.

Imagine loading a vinegar extraction of DMT on a column. Rinsing that with fresh vinegar and water, then eluting with dilute ammonia with maybe a splash of alcohol, and being done after evap. Then, to prep the column again rinse brine and water. Re-use it over and over. That would be cool I think.

Time will tell, looking forward to any input.
 
Well, running it through a column would definitely be more efficient than mixing it in the jars. When we get that far, anyway.

I feel like a wider variety of solvents should be employed though. I have seen this principle in action with pseudoephedrine pills. If it works with that, which has intentionally been made difficult to clean, surely we can make it work.

The method involved there was to dissolve In water, add alum as a flocculant, this would cause a lot of gunk to precipitate. Then, the solution was dripped through a column filled with these beads. Then, methanol and (I think) naphtha wad run through the column. And water.

Eventually they would run(in the opposite direction) brine through, which would bind to the resin and kick the pseudo off. Idk how they figured out how much resin wasneeded for a given quantity of alkaloid, but supposedly with a column set for 7 grams- in the first 2 runs 7 grams would become stuck to the resin, never to be seen again.

I wish I had better details but I never actually did it.

Hopefully I will be able to join the experiments soon. I think I will actually.

But that's my input, for now anyway.
1. Column is more efficient
2. Rinse the column while the psilocybin is bound, get rid of the hitchhikers
3. You're gonna lose a significant amount to the resin, use the same resin
4. Maybe we should try the flocculant idea.

Hoffman's method seems easier. Were these halogens not eliminated during chromatography? How problematic are they really?

Oh... I'm mostly concerned with psilocybin, A/B is easy enough in most cases. Have you tried this with the simpler molecules? I'm interested how that went
 
We did an A/B (really charged pH to isoelectronic point pH) into Xylene from water of very high ionic strength (used ammonium sulfate) and crashed out psilocin fumarate from the xylene. Yields are low thought and the process we found was cumbersome and stinky. Not practical I think.

I could be wrong of course but I'm pursuing cation resin at this time.
 
This is disheartening information. I want you to be wrong. I got very excited when I read the Hoffman extraction. So easy... I hope to get a good 20 pounds worth extracted. That should last the rest of my life, and fit nicely in my freezer

I guess I'll have to get some ion exchange resin and go in that direction. Of course it's gonna be a few months till I have any materials to work with.

Do you think psilocybin or the fumarate salt is the better idea? Obviously, we could have more alkaloids to work with if we started fresh and aimed for psilocin salts, but we are at risk of oxidation with psilocin... I didn't even knows forming a salt was even a possibility until recently. I'm still a bit skeptical.

And of course, I need to do fairly large batches for each test. I always dose at least 7 grams, so the bioassay needs that much or it's gonna seem like a fail regardless- I can barely even feel half that

Do you take any special precautions to prevent oxidation? It doesn't sound like it. If not, do you think that could be part of the problem? And what do you think about the idea of reusing the resin? It seemed to be hugely important to the other group using this method. Of course they are crazier than... well anything. They did outsmart big pharma though
 
I could very well be wrong about the Hoffman method accessibility to the kitchen alchemist, by all means, give it a shot and let us know.

To prevent oxydation/degradation I try to work in low lighting and quickly with minimal air exposure and avoid a basic pH. Folks have published that vitamin C helps during vacuum drying (but using an inert atmosphere is better). I believe we can't air dry a mushroom extract as-is since it loses a lot of its activity compared to when it is fresh and in solution. I've also tried to use HPBCD to try to stabilize psilocin but don't have clear results yet.

Regarding the salt: we got a clear psilocin peak from benzyme's MS, along with positive bioassay by me from the powder that resulted in a Xylene crash with FASA, so the salt does appear to form. The MS data is in the forum, I can fish up if you want.

Which group are you referring to regarding cation resin reuse? Is it from the team that published the isolation of psiloc(yb)in in 2010 and 2011?
 
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