psilocybin extraction/tincture tek

[jamie]

I would like to grow a large batch and try this..though I have no idea where I would get chloroform..

Also nen I have not worked with methanol..is the lye soluble in methanol? Are you filtering off the lye in the last step before you evaporate?

 

[rOm]

Yeah, we need to get onto this. Jamie, do it !

 

[nen888]

I would like to grow a large batch and try this..though I have no idea where I would get chloroform..

Also nen I have not worked with methanol..is the lye soluble in methanol? Are you filtering off the lye in the last step before you evaporate?

..chloroform from lab supply companies, but i think any halogenated solvent (dcm, xylene, hexane, limonine) should do..
..i'm not a chemist, but the only way i've been able to get methanol basic is to add lye mixed with a small amount of water..it dissolves in the water which becomes soluble in the methanol..a lot of water could degrade the psilocybin..i'd be chuffed if a chemist knows another way of basifying methanol..
.
Electric Kool-Aid wrote:

Oh man! This will be a breakthrough if you guys can come to a success of this extraction of mushrooms to smokeable base! Imagine hitting shrooms as a quick DMT like high lasting 10-20 minutes but intense like DMT! Excited beyond words, as I have looked up that extraction and was excited by the thought quite some time ago.

..yeah, it'd be quite a breakthrough, pun intended..the duration smoked is a little bit longer than DMT..

 

[endlessness]

This is interesting, I might try this sometime and see what I come up with.

One note though, xylene, hexane and limonene arent halogenated, but DCM / chloroform are. But yeah maybe defatting with some other solvent would work, who knows, we need more experiments

 

[nen888]

..thanks for that clarification endlessness..i would really like to have more data on what the advantages/disadvantages or different NP solvents (halogented or otherwise) are..that would be a helpful thread..i've always substituted dcm where chloroform is suggested in papers, and gotten good results..
..as you say, the non-polar solvent stage is for defatting..
in my one slightly crude attempt either this stage (or the actetone stage, can't remember) got out a big amount of waxy putty which had that naseua inducing quality some P. cubensis has..

 

[Nicita]

Hello fellow Nexians!

I was thinking about an cheap and easy possibility to use leftover mycelium, for example pf-Tek cakes after the last flush. Here (2nd entry) Shulgin states: "The isolation of psilocybin seemed to be quite reasonable. This alkaloid is reasonably soluble in boiling water from which it can be nicely crystallized."

Based on this statement I was thinking about grinding up a rather big amount of mycelium, extract it in acidified boiling water, filter it, extract another two or three times, then collect and reduce the solution on a low flame.
Then dissolve salt until saturated, basify and crystallize in the freezer...

Are there objections with any of these steps? As soon as I am confident that it might work, I will try it out and of cause publish the results here.

edit: I just saw that there is a subforum for extractions of non-NN-DMT tryptamines... Could someone move the thread please?

 

[benzyme]

Shulgin states: "The isolation of psilocybin seemed to be quite reasonable. This alkaloid is reasonably soluble in boiling water from which it can be nicely crystallized."

shulgin neglected the presence of proteins in psilocybe mushrooms, which can also be precipitated out of water and alcohols. the so-called "crystals" are not crystals at all, and this is realized once they're filtered and dried.

 

[nen888]

Shulgin states: "The isolation of psilocybin seemed to be quite reasonable. This alkaloid is reasonably soluble in boiling water from which it can be nicely crystallized."

shulgin neglected the presence of proteins in psilocybe mushrooms, which can also be precipitated out of water and alcohols. the so-called "crystals" are not crystals at all, and this is realized once they're filtered and dried.

..the chloroform/acetone stages of the 'Hoffmann method' posted earlier remove fats/proteins..

ps moderators, i agree with Nicita it would be good to move this thread, maybe to Psilocybin/Mushroom sub-forum..?

 

[Nicita]

shulgin neglected the presence of proteins in psilocybe mushrooms, which can also be precipitated out of water and alcohols. the so-called "crystals" are not crystals at all, and this is realized once they're filtered and dried.

Proteins are soluable in water because they are coated in a water molekules. Adding an sufficient anoubt of ions removes this coat and the proteins precipitate. Therefore a hot filtering of the salted solution should remove proteins while keeping the psilcybin in solution. Or am I mistaken here? Fats should not be a problem once crystallization can be realized...
The psilocin will stay in the material and probably be broken down by the heat while boiling. Nethertheless I think an easy method for some extra psilocybin from leftover mycelium with just water as a solvent should be possible and would be a great experiment. I am currently wayting for the last flush of two more cakes. Once these are dried I will see what I can accomplish. The mycelium also has a resonable blue staining, indicating quiet some potency.

 

[benzyme]

shulgin neglected the presence of proteins in psilocybe mushrooms, which can also be precipitated out of water and alcohols. the so-called "crystals" are not crystals at all, and this is realized once they're filtered and dried.

Proteins are soluable in water because they are coated in a water molekules. Adding an sufficient anoubt of ions removes this coat and the proteins precipitate. Therefore a hot filtering of the salted solution should remove proteins while keeping the psilcybin in solution. Or am I mistaken here?

yes you are.
shulgin mentioned nothing about acid/base chemistry when he said that, which opens a whole other
can of worms. try it, and you'll see why. psilocybin has four pKa's and the hydroxyl at position 4 of psilocin becomes an oxyanion upon basification. the way to crystals is chromatography, not a simple crystallization with a couple solvents

 

[nen888]

shulgin neglected the presence of proteins in psilocybe mushrooms, which can also be precipitated out of water and alcohols. the so-called "crystals" are not crystals at all, and this is realized once they're filtered and dried.

Proteins are soluable in water because they are coated in a water molekules. Adding an sufficient anoubt of ions removes this coat and the proteins precipitate. Therefore a hot filtering of the salted solution should remove proteins while keeping the psilcybin in solution. Or am I mistaken here?

yes you are.
shulgin mentioned nothing about acid/base chemistry when he said that, which opens a whole other
can of worms. try it, and you'll see why. psilocybin has four pKa's and the hydroxyl at position 4 of psilocin becomes an oxyanion upon basification. the way to crystals is chromatography, not a simple crystallization with a couple solvents

..as mentioned before Jim DeKorne reported a blue-grey 'crystal' (in inverted commas because it's still crude) using the Hoffmann method..sure, chromatography would be the only way to get pure psilocybin crystals, but de Korne's extract was pure enough to have good effects vaporized..

 

[Nicita]

Okay, I will forget about crystals right now. Regardless of that I will try to make consumable extract from the mycelium using water as solvent.
The information that psilocybin is only soluble in boiling water is right? If this is the case, I want to make a few washes of the powdered mycelium with dem. H2O before the extraction. Should I expect a lose in psilocybin yield with this method? Has anyone tested the solubility of psilocybin crystals in cold H2O? This process should wash many of the carbohydrates and proteins highly soluble in water. The dem. H2O should also lyse the cells that are not broken down by pulverizing due to the osmotic pressure.
If this wash idea is nonsense I will limit myself to extracting with boiling water for several times. I still can purify with acetone and chloroform washes or get an easy column chromatography setup for further extractions if the bioassay satisfies me.

 

[obliguhl]

The information that psilocybin is only soluble in boiling water is right?

I just got the idea to soak the cakes in lemon juice to make a strong lemon tek tea.
What would happen if one would evap the lemon juice down? I think this question has been posed before. Perhaps one could alos conservate the psylocin afterwards with alcohol.

 

[benzyme]

proteins highly soluble in water.

you're not understanding something...the proteins are not soluble in water, because they precipitate with the alkaloids, resulting in a residue that turns green. compounds will precipitate when they are insoluble in a solution

 

[benzyme]

shulgin neglected the presence of proteins in psilocybe mushrooms, which can also be precipitated out of water and alcohols. the so-called "crystals" are not crystals at all, and this is realized once they're filtered and dried.

Proteins are soluable in water because they are coated in a water molekules. Adding an sufficient anoubt of ions removes this coat and the proteins precipitate. Therefore a hot filtering of the salted solution should remove proteins while keeping the psilcybin in solution. Or am I mistaken here?

yes you are.
shulgin mentioned nothing about acid/base chemistry when he said that, which opens a whole other
can of worms. try it, and you'll see why. psilocybin has four pKa's and the hydroxyl at position 4 of psilocin becomes an oxyanion upon basification. the way to crystals is chromatography, not a simple crystallization with a couple solvents

..as mentioned before Jim DeKorne reported a blue-grey 'crystal' (in inverted commas because it's still crude) using the Hoffmann method..sure, chromatography would be the only way to get pure psilocybin crystals, but de Korne's extract was pure enough to have good effects vaporized..

have you tried that method yet?
I've done four a/b extractions on psilocybes, from 2.5 to 10 g of biomass and various pH's below 9. the result after crystalization was a dark greenish residue that was weakly active orally.

 

[Nicita]

proteins highly soluble in water.

you're not understanding something...the proteins are not soluble in water, because they precipitate with the alkaloids, resulting in a residue that turns green. compounds will precipitate when they are insoluble in a solution

I don't want to precipitate. The current plan is to extract and then evaporate the water. That yields of cause many impurities and my idea to reduce them was to wash with cold water before extracting with boiling water. This would wash out sugars, other carbohydrates and water soluble proteins (the ones that are also soluble in cytoplasm). Of cause this would only work if psilocybin is reasonable insoluble in cold water and the wash would not reduce the yield by a significant amount. This is the reason I asked if someone knows the solubility of psilocybin in cold water.

 

[benzyme]

lol that's not going to separate out anything, but try it so you can see for yourself

xD

 

[Nicita]

Thats probably the best I'll post some pictures and reports of bioassay. :lol:

 

[Doodazzle]

Nicita...you've been both lol'd and XD'd. Yet still you proceed? The universe may just reverse it's habits or laws temporarily to reward your pluck.

 

[Shaolin]

Nicita...you've been both lol'd and XD'd. Yet still you proceed? The universe may just reverse it's habits or laws temporarily to reward your pluck.

Testing a hypothesis is never without value as long as one keeps notes.