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Psilocin extraction help

Migrated topic.
i'm still pondering how it can be salvaged..

what i was concerned about earlier is this:

the sugars and structural proteins are bound to the psilocybin, but also probably to the fats..
(and the psilocybin (being a zwitterton) is partially bound by both salt and base..its a complex joining together going on in there)

i assume there's a reason the chloroform defat in the Hofmann procedure precedes the acetone wash..
sometimes what seems simple has a quite advanced reasoning behind it..

i would guess that the fats may need to be dislodged first, to 'expose' the structural proteins properly to the acetone, which after dislodging them, exposes the alkaloids to the methanol

also, the other possible issue relates to what i meant when i said acetone will behave differently with even just 1% water (a couple pages back) ..by this i meant that i suspected that the psilocybin would become more soluble in that case, and be lifted..

the procedure itself emphasises at the start, that success is dependant on the level of dryness in the material..so finely powdered does help..but what i'm getting at is the acetone (having slight water content via mushrooms still) could possibly lift the alkaloid along with sugars..it did look like the evap crystals were water..

doing the defat first with an NP solvent would further help reduce residual water content..

if the three different fractional residues were combined, the procedure could be theoretically 'mini-repeated'..

anyhow...this is my guess what may have happened..i'm not an advanced chemist though..
and bound sugars will render alkaloids really unsuited to pyrolysis.. ..the end result should be fairly dense

if you can get this bit to work, then it 'works' (by vaporisation)
 
i havent forgotten this thread.
still in the middle of massive rebuild dentistry.
im avoiding solvents this month.

im still with NEN888 on this....
( cept annie style variants)

wheres steppa?
 
Haven't got time really to explore this ATM, might come back to it over Easter. Still think the alks might be in there, just not smokable? Need to try oral. Otherwise they might just be in one of the two solvents?

Not sure about the crystals being water... It was about 12 degrees and it only happened with the DCM, not acetone. The mushrooms were dried well, and although it's possible that a small amount of condensation occurred after drying, surely the acetone would have pulled that since they're miscible?
 
wheres steppa?
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He's here for sure. 😁

And he's willing to post the procedure you walked him through. Although he thinks that his experiment was far from beeing sucessful. He thinks it was a failure. (= not worth showing off)

He can post the rundown (with pics) of what he did nevertheless, if you want him to. It would be much cooler to present a success story, though.

But we'll have to wait a bit for that. New shrooms need to grow first...but he already has got that going for him, which is nice. :)

But honestly he's torn between giving your method another try and trying another method (by ion) combined with your method of washing the shrooms first.
 
anne halonium said:
i havent forgotten this thread.
still in the middle of massive rebuild dentistry.
im avoiding solvents this month.

im still with NEN888 on this....
( cept annie style variants)

wheres steppa?
Click to expand...

nice to hear from you anne halonium, and i hope your teeth a well..

and yeah i'm down with your technique too ;)

...

User_7..i can only guess...but if the process went normally, the end crude result should be noticeable by pyrolysis (with increasing noticeability as it approaches crystal solidity which depends on the efficiency of the procedure)
..jamie's tar sounded like it got more of the alkaloids, as he 'noticed' it at least..but there'd be sugars getting in the way...i suspect the soup's become a bit 'scrambled' and needs to be recombined and re-procedured..remember though, this would only require very small amounts of solvents, compared with the initial extraction..my instinct says the defat has to precede the acetone..as sayeth the tek of hofmann..good luck
...


if i think about it...if you want a 'holy grail' of alchemy, a true high art extraction achievement..
then you have psilocybin
(as opposed to psilocin)
and yes psilocybin is the stable one..

this Humito is, for the 'mushroom camp' lol, like the fire of the soma

the cows are part of the plot haha

a challenge and art form for alchemists for many ages..
.
 

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The wet slime is active orally, or at least lingually! After the failed smoking experiment I left a small amount of goo which wasn't caught by my scraper on the plate. The plate has just been knocking around since then waiting for me to rinse it back in with the rest. But as I was clearing up today I thought I might as well just lick it up and see what happens. Carried on cleaning and forgot about it. Suddenly I feel it now. In my body more than anything but also altering my perspective. Unmistakable. I found it a little hard to navigate hear and write this message. Couldn't really read yours nen. No visuals but bear in mind this is only what was too close to the plate to get scrapped from 2.8g equivalent.

Unfortunately what I feel in my body is largely what I was hoping to pull away with this extraction, but I do believe it is just part of the psilocybin experience for me, no matter of purity. Kind of like low dose DMT onset but more squirmy. No nausea but can imagine the feeling manifesting itself as nausea in a full dose, further experiments needed.

For this small of a dose to be active I think there must be negligible alks in the acetone and DCM. So The reverse Hoffman works, but perhaps it pulls some extra crap this way around and that's why our extracts look different. Or perhaps if I evaporated a bigger batch and dried away any moisture (possible water?) it might be more crystaly?
 
So The reverse Hoffman works, but perhaps it pulls some extra crap this way around and that's why our extracts look different. Or perhaps if I evaporated a bigger batch and dried away any moisture (possible water?) it might be more crystaly?
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..well...reversing it i don't think has worked any better than jamie's simple extraction...and i think you could get a similar or better result simply using methanol, as benzyme did..it may not be water moisture making it not crystally..there's other stuff..also, without knowing in mg how much you had is hard to estimate, but if it's with approaching pure psilocybin, 10mg should be very 'noticeable', which is like a small match-head, or less

it's good that you've got something so far, but if the Hofmann method has 'worked' it should be noticeable by pyrolysis (if just as a test of purity), and should range from a purple/brown semi-solid gunk/wax to a blue-grey crystal wax as it get's purer..
blue-grey-brown-purple...that's psilocybin (& alks)

that wasn't simply 'my' result by the way...Jim De Korne (founder of ER) reported similar..as have a few others..the pure psilocybin crystals pictured above were done by Jeremy Bigwood, using chroma...
 
Evaporated the other solvents. Acetone yields a wet mostly green slime with some bluish grey patches, red tones in places and also some yellow. Mild sweet smell. DCM yields blue/grey waxy substances, with some yellow bits and a stronger sweet smell like the methanol product. I'm thinking the blue is psilocin derived oxides?

I dabbed a small bit of each and noted that neither are at all bitter. In contrast the methanol product was very bitter. Bitterness makes me think alkaloids. I would be really interested if anyone can comment on whether or not their extracts were bitter? Or if they happen to know if psilocybin would taste bitter?

Top pic is acetone residue, bottom from DCM:
 

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Nen, by suggesting I could perhaps get a better result with a simple methanol extraction, are you suggesting greater efficiency? Because I can't see how just using methanol could result in a cleaner product, clearly my washes have removed quite a lot of stuff and that could only have reduced the purity of the end product if not done before hand. The only way I see that they could have been of detriment is if they have pulled some of my actives. I'm not suggesting that my product is particularly pure, but it is surely purer than a simple methanol extraction?

Regarding how much I consumed. No, I don't know in mg, but if you go back a page to the pic of the scraped up goo, that is 2.8 dried gram equivalent on a small side plate. What is scraped up in the middle plus what I could mop up around the sides was smoked. You can see how little would have been left for me to ingest, a really thin film on a small plate, with definite effects. I'm thinking if I used a little heat to dry off the moisture It might be more crystalline, maybe water had condensed on the plate during evap giving it that wet sliminess. This water may have stopped it smoking effectively.

Going to order some glycerine and try vaping it.

Also looking forward to hearing back from you Annie. Plus anyone who can comment on bitterness!

So far a few dabbles of the acetone and DCM products are inactive :thumb_up:
 
Evaporation residue from methanol extraction can be bitter if the methanol you used contains bitrex. It is not uncommon for OTC methanol to contain adulterants like bitrex, this is done to discourage accidental or uninformed ingestion.

You should make sure to correctly dry and distill your methanol and acetone before use. Also make sure that the mushrooms you extract are thoroughly dried. Mere air drying is not good enough. You can air dry the mushrooms initially when fresh and wet, but when the bulk of water has evaporated, the mushroom bodies should be dried over anhydrous calcium chloride in an airtight container in a cool and dark place. Properly dried mushrooms easily crumble to powder when lightly pressed or squeezed.
 
My methanol claims 99.95% purity and lists no additives on the bottle. Surely they'd have to state that it contains anything else?. Aren't most tryptamines bitter?

The mushrooms were dried with gentle heat and surrounded by silica gel sachets, then stored in air tight jars with more dried silica gel sachets. That being said, they still retained some strength and didn't powder completely so I'll definitely give calcium chloride a go next time. Or perhaps magnesium sulphate would substitute, as I already have this?

I was also a little sloppy for opening cold jars before it occurred to be that moisture would condense on my mushrooms. Then when evaporating my methanol and acetone, I imagine they pulled moisture from the air before they evaporated, leaving it on the plate.
 
User_7 said:
My methanol claims 99.95% purity and lists no additives on the bottle. Surely they'd have to state that it contains anything else?. Aren't most tryptamines bitter?
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If items are not meant for consumption, the rules for listing ingredients are less strict. Bitrex needs only be present in parts per million, so even 0.05% bitrex would be a lot. Note that I am just speculating about the bitrex, but I've personally seen "pure" methanol that contained bitrex. Unless you have reagent or analytical grade methanol from a chemical supplier, accompanied with analysis certificates, don't assume too much about purity.

User_7 said:
The mushrooms were dried with gentle heat and surrounded by silica gel sachets, then stored in air tight jars with more dried silica gel sachets. That being said, they still retained some strength and didn't powder completely so I'll definitely give calcium chloride a go next time. Or perhaps magnesium sulphate would substitute, as I already have this?
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In my experience, silica gel is not as good as calcium chloride. I guess magnesium sulphate is okay too (but heat it strongly to get all the water out). It's because calcium chloride is so easily and cheaply available that I do not bother with baking magnesium sulphate. For drying your solvents, use the anhydrous magnesium sulphate though. Calcium chloride is not good for that. You can use the silica for storage after the mushrooms have been thoroughly dried. Its main advantage is that it will not deliquesce and melt into the shrooms when it exceeds its moisture absorption capacity, like the salts can do. If you use a properly calculated amount of calcium chloride, that should not have to be a problem.
 
Hey,

I'm now in a position to think about another extraction approach again.

My current plan looks like this:

- Powdering bone dry, crispy mushrooms to flour like consistency.

- Blasting some shit out ouf them with butane

- Re-drying the powder and then following this instruction from the nook:

Seal the powder in a jar (make sure the level of the powder is AT MOST only half the volume of the jar) and freeze it until you are ready to use it. Refrigerate some methanol. Take the jar of powder out of the freezer... QUICKLY open the methanol jar, then the powder jar, and swiftly add the methanol to the powder about an inch (small jar) or half inch (large jar) above the level of the powder, and QUICKLY seal the mixture jar.
*I say "quickly" because cold jars will gather water condensate from the surrounding air... this will mix with alcohol... this will really suck later. It is best to do all of these procedures in a dessicated glove box (just a bowl of Ca chloride set in the glove box for an hour prior to work).*

Swirl this slurry (methanol+powder) around for about half an hour, relieving pressure every couple minutes (warming alcohol will expand gaseously, so pressure relief is necessary for safety, though I doubt the jar will actually pop or anything...). Let the slurry settle and pour the alcohol through a funnel, filtered by either:
a. vacuum filtration through filter paper (this may clog, though)
b. a layer of dense fabric (high knit sheet or shirt) with a coffee filter on top. This will be squeezed to remove last liquids.

The leftover crud (filter cake) can be extracted by repeating the methanol extraction outlined, or it can be thrown out. You will probably want to re-extract the first few times, until you get the hang of doing this perfectly.

Evaporate the methanol by blowing over the jar with a fan... this, too should be done with dessicated, de-oxygenated air, but the apparatus is too complex to build for description here... it may be in my kitchen chemistry chat posts ??

As you evaporate, you MAY see crystals... maybe not. Either way, continue evaporating to dryness.

This residue may be eaten in doses of about 3 times that you would take of pure psilocin (30mg residue = 10mg psilocin)... this depends on the strength of the shroom (that's why crystal would be better, because you would KNOW how much goodie you are eating). If you have crystals, just measure them directly as weight of psilocin.

BTW, this is a mixture of psilocin and pilocybin... I only say psilocin for the sake of brevity, in that psilocin is the more potent molecule by weight. Most of the mix will be psilocybin, but it is better to err to the lower end of dose.

Here's the big trick to decent purification of these compounds:
Dissolve the residue and/or impure crystals in room temp. petroleum ether (in this case, you can use zippo fluid). You may notice that crystals don't dissolve well, though they might (because of impurities). Only add enough pet. ether to get the stuff suspended/dissolved as you stir... if crystals won't dissolve, DON'T add more pet. ether. Crystals not dissolving is GOOD!

Close the container you are doing this in and put it in the fridge. When it gets to fridge temp, put it in the freezer. (Slow cooling forms bigger crystals ). Leave in freezer until you see no more crystal growth (overnight, usually).

Stir up the mix (still freezing cold) with a cold stirring rod, suspending the crystals in the liquid. Swiftly pour this into the vacuum filter apparatus and flip it on. Rinse the container with a bit of more freezing cold pet ether, and dump this into the filter. You want to get every last crystal, right?

Leave the vacuum on until the crystals are dried by the air (again, preferably dessicated and de-oxygenated). This is a relatively pure crystalline mix of psilocin and psilocybin.

Depending on experience and perfectionism, the yeild from a single methanol extraction (no re-extraction of the mushy filter cake) of this caliber is approximately 95%. Most losses occur from oxidation, over use of solvents, bad temperature control, and transfers (leftover drops in containers).

To store this pure product, get some pure ascorbic acid (vitamin C) crystals. Dissolve some of the vit. C in twice it's volume of 190pf ethanol. Now, dissolve your cin/cybin crystals in this acidic ethanol.

Put this mixture in a dark container (something opaque) in the freezer.

That's it!

-ion
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Does this look about right? At least they look exactly like in the first pic nen posted on this page. They are still floating in NPS. What's the smartest way to get them out without loosing too much?
 

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