• Members of the previous forum can retrieve their temporary password here, (login and check your PM).

Recrystallizing Psilocybin

Migrated topic.
4

4-HO-DMT

Rising Star
Will psilocybin dissolve in hot n-heptane, or light petroleum ether? I feel like there should be some way to recrystallize the crude extract.
 
No, you can defat with them, but more polar solvents are a better choice to recrystallize. Psilocybin can be recrystallized in destilled Water, 70% Alcohol, 95% Alcohol, Methanol etc

Best to go with the alcohols, I've had troubles with honey-like goo using water.
You can precipitate Psilocybin from dry (!) Ethanol, (pre-drying the solvent with magnesium sulfate or similar)
 
Fractional precipitation with dried Ethanol. Doesn't yield pure Psilocybin though, pure enough if you do it right, no gunk nice crystals, but timing is pretty important so not recommended for beginners for proper batches. Easy enough to do for recrystallizations though.
 
I've always wanted to extract psilocin/psilocybin, I've read how Hoffman did it and how other people have tried on here, do you have a guide or procedure on how you do it, volumes to use ect

Thanks
 
Crystal extraction has been discussed here many times before. So far, I've never seen any evidence that you could get a pure product (>95%) with anything short of column chromatography. Freebase psilcoybin doesn't exist, and while you can evaporate ethanol extracts, you're still going to get a lot of gunk contaminating your product (mushroom proteins and enzymes bound to the actives, iirc) .

Unless there's been some serious chemistry done in the last few years I'm unaware of.
See this thread for details.

Blessings
~ND
 
Here this might be helpful.

As I said my own method isn't very useful for beginners, because if you don't do it right, you would be getting exactly the same result like when you just soak some shrooms in alcohol and evaporate that. Very impure & crude extract. You'd have to stay on top of it and separate the precipitate several times from the solvent at the right time to get different grades of product and have to pick the right one. As I said it gives crystals, but they're still contaminated with Polysaccharides.

To be honest I don't even do it myself anymore, not worth the effort to me, I like dry shrooms. The only benefit is that you can smoke the product, but only in low amounts, never managed to breakthrough, the complex sugars seem to get into the way somehow.
 
hermes111 said:
Here this might be helpful.

As I said my own method isn't very useful for beginners, because if you don't do it right, you would be getting exactly the same result like when you just soak some shrooms in alcohol and evaporate that. Very impure & crude extract. You'd have to stay on top of it and separate the precipitate several times from the solvent at the right time to get different grades of product and have to pick the right one. As I said it gives crystals, but they're still contaminated with Polysaccharides.

To be honest I don't even do it myself anymore, not worth the effort to me, I like dry shrooms. The only benefit is that you can smoke the product, but only in low amounts, never managed to breakthrough, the complex sugars seem to get into the way somehow.
Click to expand...
Read the thread I linked - that particular tek has been dissected many times, unfortunately, Shulgin got it wrong. Because psilocybin is always a charged compound, it's going to pull a lot of junk with it. I think analysis found that, when following Shulgin's tek, you were getting less than 50% purity. If all you want is just a solid thing you can eat, then it works fine, but when we talk about recrystalization, we're usually talking about a purification technique to yield very pure product.

Benzyme, who is our resident chemistry whizz has spoken at length about why extraction of psilocybin and psilocin is very different from DMT. The presence of the oxygen group on the indole ring changes the behavior of the molecule in some important ways.

Blessings
~ND
 
Read my posts ;) . I was just giving him what he wanted.
My method is different, dry ethanol, prolonged(weeks) denaturation + fractional precipitation. The majority of gunk precipitates first, one just has to be quick enough to remove it/change containers before the goodies follow to get rid of it. I'm not claiming analytical purity. Just less crap than the known method. As I said mostly polysaccharides that survive the process.
 
Thanks for the input guys, it's given me a lot to consider. I think chromatography is the way to go. I'll try spotting it out using TLC first. Any ideas on which eluents you can get easily that would work for this application?
 
ethanol will not dissolve/separate any structural proteins from the alkaloid, the complexes readily precipitate out of anhydrous ethanol. charge-based separation is required to get rid of the "gunk", i.e. separation of a dilute acidic solution on a bed of cation exchange resin, and elute with dilute ammonia, while gradually altering the pH. keep in mind though, dephosphorylation may occur at pH > 9, and pH < 3. solvent partitioning is another option, this is done following a series of A/B extractions.

for TLC, the eluant is typically butanol:methanol: dilute ammonia 4:3:1.5. alternately, ethyl acetate may be substituted for the methanol, and acetic acid is substituted for the ammonia.

psilocybe alks aren't very stable as zwitterions, and have the tendency to bind anything electrostatically. anionic psilocin (which is what you'll get if you basify to pH 10-12, net charge of -1) is most stable as a salt complex, preferably with an acid having antioxidative properties, i.e. maleic, or tartaric acid. this complexation would ideally occur at pH 2-3.
 
benzyme said:
ethanol will not dissolve/separate any structural proteins from the alkaloid, the complexes readily precipitate out of anhydrous ethanol. charge-based separation is required to get rid of the "gunk", i.e. separation of a dilute acidic solution on a bed of cation exchange resin, and elute with dilute ammonia, while gradually altering the pH. keep in mind though, dephosphorylation may occur at pH > 9, and pH < 3. solvent partitioning is another option, this is done following a series of A/B extractions.

for TLC, the eluant is typically butanol:methanol: dilute ammonia 4:3:1.5. alternately, ethyl acetate may be substituted for the methanol, and acetic acid is substituted for the ammonia.

psilocybe alks aren't very stable as zwitterions, and have the tendency to bind anything electrostatically. anionic psilocin (which is what you'll get if you basify to pH 10-12, net charge of -1) is most stable as a salt complex, preferably with an acid having antioxidative properties, i.e. maleic, or tartaric acid. this complexation would ideally occur at pH 2-3.
Click to expand...

Benzyme your one of the most knowledgeable people on this forum, if I wanted to do an extraction on mushrooms which is the best way to go about it, what would I need to do to get something with decent purity whether it be a resin, a powder ect
 
IEF? no.
steppa and sbc1, what you guys are interested in is the solvent partitioning...it's A/B/A/B/A, or liquid-liquid extraction with a number of solvents, and a lot of sep funnel work. but it is less complicated than ion-exchange preparative chromatography.
solvent partitioning is the approach hoffman used, it follows a flow-chart format; steppa, you used that one, right?
it's cited a few times in the psilocin extraction thread, and favored by anne.

another approach I would try is A/B through an SPE column (looks like a plastic syringe tube with silica), which typically has size exclusion resin. this may separate out the large structural and ribosomal proteins, allowing alkaloids (small molecules) to elute. then add alcoholic tartaric or maleic acid solution to the eluent, and freeze precipitate.

but first, check the pH range specifications of the resin
 
What would be so difficult about using an ion exchange resin? Is there a detailed procedure in the literature or somewhere on the Nexus?
 
it'll be mostly trial and error.
IEX chromatography involves gradually changing the pH gradient, or salt concentration. for the purpose mentioned here, pH gradient is relevant.

it is a technique mainly applied to separation of proteins in an HPLC setup, but could also be applied on the preparative scale, to isolate small molecules. I've mentioned it in a few threads, for psilocin and lysergic acid isolation, mostly as an idea for extraction methods.
 
So only a certain ph will be able to remove psilocybin from the cation exchange resin, and we don't know what that ph is? Or is there something about the change in the ph itself that I'm not understanding?
 
honestly, I'd suggest getting some SPE columns from e.bay, and practice doing A/B through those; i.e. grind your material, acidify it and let sit in a hot water bath at 50C for half an hour, filter, pour solution through the SPE column to saturate it, and pour dilute ammonia (pH 9-10) through it. extract with ethyl acetate or dcm, salt with alcoholic tartaric acid.

to regenerate the columns, pour saturated saline solution through them.
 
Back
Top Bottom