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Psilocin extraction help Options
 
User_7
#1 Posted : 2/7/2016 12:24:55 AM

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Hi guys, waiting for approval to post this in a chemistry forum, but until I get enough votes it was suggested that I just post it here. Please do vote me up in the mean time, you can read briefly about me here.

Anyway, I'm a long time Shroomery member and this is just a paste from my thread there which wasn't getting any answers. I know there's some fine chemists here.

I was lucky enough to find a roundabout covered in Psilocybe cyanescens late this season. Needless to say it is now known as the magic roundabout. After cleaning and drying my pickings they came to exactly 1oz. They are currently in an air tight Kilner style jar in my freezer.

My goal is to create a potent extraction which will store well in the freezer. Purity isn't a big issue but it's essential to leave out the nauseating and squirm inducing nasties. One important thing to note is that the species I am working with is much higher in the more fragile molecule psilocin, than its cousin psilocybin. As well as impacting stability I understand this will affect my choice of solvents.

So I'm looking for guidance on how best to approach the extraction and create a reasonably stable product. I've read mostly about 3 solvents so far:
- methanol is great for psilocybin but rubbish for psilocin, so probably only worth while for a second pull.
- ethanol is rubbish on it's own, but great with 30% water. My concern then is that the nasties will dissolve in the water, which I don't want, do you think this is a reasonable fear? Also hard to obtain high proof in the UK.
- 5% acetic acid (vinegar) is supposedly great, but again, at 95% water, I'm worried it's just going to take all the crap with it and be as nauseating as tea? Or does it not work like that?
Don't know much about isopropyl alcohol or other solvents, but would love to hear!

Then storing the extraction. If I used 70% alcohol or vinegar I'd be worried the water would degrade my alkaloids. And if it's in anything else I can't ingest it without having to evaporate it. Was thinking of adding ascorbic acid (vitamin c) as a preservative, could I store in frozen water with antioxidants?

Also interested in extraction temperatures and time to maximise extraction but minimise psilocin degradation. Overall a clean trip is more important than getting 100% of the alkaloids.

Cheers in advance
 

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User_7
#2 Posted : 2/7/2016 12:49:17 AM

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Inderstand that an A/B extraction isn't likely to work well because psilocin is amphoteric, so currently I'm leaning towards the %70 ethanol soak. Then maybe wash with solvents to get rid of nasties (peptides?). Hopefully in the freezer it will be stable with vitamin c, despite %30 water. Or maybe I could dry it with epsom salts or something? Do you agree that it'd be more stable in that than 5% acetic acid?

One problem is acquiring %70 ethanol. I can get %95 ethanol which isn't denatured and dilute it. The seller assures me there's no additives it's literally %95 ethanol %5 water, but it's not sold as potable. Do you think it'd be safe to consume a few drops as a tincture diluted in a juice, or is the lab stuff distilled from something different to potable alcohol like Everclear?

 
sbc1
#3 Posted : 2/7/2016 12:57:37 AM
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I'd love to hear some responses to, try spirytus it's 95% drinking alcohol and you can buy it in the uk it's polish vodka although it's pretty dear nearly £30 a bottle
 
anne halonium
#4 Posted : 2/7/2016 8:03:45 AM

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we just use vodka,
as seen in the " annie oxidation" thread .
https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=63716
"loph girl incarnate / lab rabbits included"
kids dont try anything annie does at home ,
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User_7
#5 Posted : 2/7/2016 10:39:47 AM

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Yeah, I've come across spirytus online, but don't have a Polish shop around unfortunately. And it is a lot more pricy than the ethanol.

Annie, do you find your extraction lasts well in the vodka? Also do you notice much difference in body load versus eating the fruits strait or making tea?

I have very bad nausea and restless limbs from mushroom tea, which distracts me from the wonders occurring before my eyes. I'm worried that at %50 water, I'll pull the same nasties. Thinking of a naphtha wash + maybe some other solvents to try clean it up a bit.
 
Mindlusion
#6 Posted : 2/7/2016 3:19:32 PM

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Yeah don't use vodka, the water will pull unnecessary gunk will rehydrate the the cells giving you a gunky mess.

The liquid tincture should store pretty well in the freezer though.

Your best bet is probably methanol, psilocin is very susceptible to oxidation, especially in solution (as well pointed out by annie in her demo!). If you want an extract to store for any length of time you will be looking at psilocybin. Which isn't really a big deal, they contain mostly psilocybin. You just need to remove the methanol quickly and completely, without applying too much heat.

I don't see why 95% ethanol wouldn't be suitable, it will definitely pull the alkaloids. The small amount of water won't be a big deal, it just will slow down the evaporation. But perfect if you are after a tincture.

The biggest obstacle seems to be you have to work fast to get a good product, filtering the mushroom pulp can be a pain. And ethanol is harder to evaporate than methanol. You could get away with sticking it in a dry dark room with a fan for a few hours. This extraction works really well if you have proper tools, vacuum filtration to filter quickly and cleanly, rotary evaporator to remove the solvent quickly under vaccum without applying any heat.

Also, it may not be the the gunk in mushrooms causing you nausea. Tryptamines THEMSELVES cause nausea. Some people tend to be more sensitive than others. But, then again, it could also be your stomach disagreeing with the poor digestion of the fungus. So worth a try definitely.
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PsyDuckmonkey
#7 Posted : 2/7/2016 4:42:59 PM

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User_7 wrote:
I have very bad nausea and restless limbs from mushroom tea, which distracts me from the wonders occurring before my eyes.

As in mushroom tea in general (including Cubensis tea), or just Azurescens tea? I'm asking this because they say Azurescens specifically contains some disagreeable compounds, and may cause negative body effects.

I never had any problems with Cubensis if I chewed it enough before swallowing. The lemon cocktail has given me some mild nausea, but it could have just been the undiluted lemon juice.
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Biawak
#8 Posted : 2/7/2016 7:47:16 PM
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One could try a chloroform or DCM soak/filter/discard and then an acetone soak/filter/discard before extracting with ethanol.
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downwardsfromzero
#9 Posted : 2/8/2016 6:13:10 AM

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I never got problems with nausea from cyanescens; I'd say anything other than sticking them in vodka in terms of processing is a waste of time.

Even the vodka's not necessary, why not just stick soup in the freezer? Keeps reliably for two years, you know?

Otherwise just dried and powdered, kept in something airtight in the dark. Maybe with a silica gel packet.


Otherwise you're talking acetic acid, ammonia and butanol for the extraction.


Regarding high proof ethanol, why not distil your own? It's not as if it's any more illegal than what you're already proposing Very happy
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PsyDuckmonkey
#10 Posted : 2/8/2016 10:21:32 AM

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downwardsfromzero wrote:
Regarding high proof ethanol, why not distil your own? It's not as if it's any more illegal than what you're already proposing Very happy

Haha, good old moonshine, the illegal drug op of my grandfather. Smile I still have his still stuffed away somewhere.
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User_7
#11 Posted : 2/8/2016 8:24:29 PM

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Mindlusion wrote:
. If you want an extract to store for any length of time you will be looking at psilocybin. Which isn't really a big deal, they contain mostly psilocybin. You just need to remove the methanol quickly and completely, without applying too much heat.

Oh yeah, I was thinking they contained more psilocin than psilocybin. But I see now that you're correct and psilocybin is the main psychoactive constituent. Must have been confused with them having more psilocin than P. semilanceata. This would suggest methanol is suitable.

Mindlusion wrote:
I don't see why 95% ethanol wouldn't be suitable, it will definitely pull the alkaloids. The small amount of water won't be a big deal, it just will slow down the evaporation. But perfect if you are after a tincture.

Apparently straight ethanol doesn't pull them very well. Here's Shulgin saying that.


Mindlusion wrote:
Also, it may not be the the gunk in mushrooms causing you nausea. Tryptamines THEMSELVES cause nausea. Some people tend to be more sensitive than others. But, then again, it could also be your stomach disagreeing with the poor digestion of the fungus. So worth a try definitely.

Yeah, I'm not entirely sure, I've just heard a lot of people say that extractions give less nausea, so want to try it. I'll go into that in a little more detail in a minute.
 
User_7
#12 Posted : 2/8/2016 8:56:13 PM

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PsyDuckmonkey wrote:

As in mushroom tea in general (including Cubensis tea), or just Azurescens tea? I'm asking this because they say Azurescens specifically contains some disagreeable compounds, and may cause negative body effects.

I've only ever tried Psilocybe cyanescens and semilanceata. Always as tea, sometimes with lemon and ginger and cyans only in combination with semis. Every time all participants report nausea and body load. Two participants had previously tried cubensis and unidentified mushrooms in Indonesia which I suspect to be Panaeolus cyanescens with no ill effects, so not sure if it's just something in our slimy English mushrooms. One user also reports having since tried a semilaceata extract with zero negative effects.

Also I've read loads of reports on the internet of people saying extracts reduce body load, nausea and generally give a cleaner trip.
 
User_7
#13 Posted : 2/8/2016 9:08:55 PM

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Biawak wrote:
One could try a chloroform or DCM soak/filter/discard and then an acetone soak/filter/discard before extracting with ethanol.

This is the kind of thing I was after. Not sure how practical chloroform is though. How sure are you that psilocybin/psilocin won't dissolve in DCM and acetone?

But now Mindlusion pointed out that Psilocybin will be my primary alkaloid, I'm thinking of just doing a couple of methanol pulls. Then evaporate and dissolve in vodka or something just to store. Do you think the extracted Psilocybin will dissolve Ok in vodka since ethanol isn't really a suitable solvent to extract it with? Or if it won't dissolve, do you think it will store OK as crystals in the bottom?

downwardsfromzero wrote:
Otherwise you're talking acetic acid, ammonia and butanol for the extraction.

Do you have further details on this process or a link to a tek?
 
nen888
#14 Posted : 2/9/2016 12:54:06 AM
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from https://www.dmt-nexus.me...=302926&#post302926

Quote:
Le Genre Panaeolus: Essai taxinomique et physiologique par Gyorgy Miklos OLA'H Laboratoire De Cryptogamie du Museum National D'histoire Naturelle 12, rue de Buffon, Paris. Memoire hors-series No 10, 1970. Page 97.

Dry the mushrooms.
This important step is most likely to cause the greatest loss of yield depending on how it is done. Crush or grind the dried carpophores or mycelium to a powder.
Shake and allow to stand (e.g. 30 mins) in chloroform. Use maybe twice the dry weight in solvents at every step, or enough to well cover the powder.
Filter and discard the chloroform.
Shake the reidue and allow to stand with acetone.
Filter and discard the acetone.
Shake residue and allow to stand with methanol.
Filter.
Shake residue and allow to stand with methanol.
Filter.
Shake residue and allow to stand with methanol.
Filter.
Discard residue.
Combine methanol extracts.
Evaporate methanol to dryness, preferably in a vacuum, although low heat will do.

This will yield a crude extract containing the active tryptamines, suitable for most purposes. This can be further chromatographed on cellulose etc. to give pure psilocin and psilocybin. The recommended solvents are n-Butanol saturated with water, and n-butanol:acetic acid:water (24:10:10). Anyone wishing to do chromatography should check the relevant texts for more detailed instructions.


 
Mindlusion
#15 Posted : 2/9/2016 1:41:33 AM

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Mindlusion wrote:
I don't see why 95% ethanol wouldn't be suitable, it will definitely pull the alkaloids. The small amount of water won't be a big deal, it just will slow down the evaporation. But perfect if you are after a tincture.

Apparently straight ethanol doesn't pull them very well. Here's Shulgin saying that.H

Heh, pure psilocybin crystallizing out of the 95% ethanol during a soxhlet extraction? Count me in! I may give that a try.
Expect nothing, Receive everything.
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Biawak
#16 Posted : 2/9/2016 3:25:40 AM
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The Hofmann method posted above is where I got that. Not really a mushroom guy, so I've never actually tried any of this.

Chloroform is super easy to make. DCM can be distilled easily from paint stripper in the US. Not sure about the UK.

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User_7
#17 Posted : 2/9/2016 1:50:50 PM

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Mindlusion wrote:

Heh, pure psilocybin crystallizing out of the 95% ethanol during a soxhlet extraction? Count me in! I may give that a try.

I actually read someone saying that Shulgin was incorrect to assume that would yield pure psilocybin. Think it was somewhere on nexus. Still, might be a good method for a reasonably clean product. Guess you could estimate purity from the weight of crystals you get out of x grams of mushroom - if the psilocybin is pure it'd be a tiny fraction of the weight.

Chloroform just seems dauntingly toxic. Can buy DCM here though.

Think for now I'll just do a methanol pull and if the product is still nauseating I'll wash it with DCM and acetone and see if that cleans it up.

Would still be interested in a vinegar method though if anyone knows any good details? But I'm worried the PH and water content will lead to rapid degradation. Maybe I'll save the mushroom sludge after the methanol pull, then try a vinegar pull to get the psilocin the methanol left behind. If it works I can then add vitamin c, freeze and retest to see if it retrains potency myself.
 
anne halonium
#18 Posted : 2/9/2016 6:50:14 PM

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there are ways to do this..........

but think about it, any actual workable reliable scale extraction,
might be too hell raising for this forum.

keep in mind, its a zwitteron.
so it doesnt act like a regular alk we love........
"loph girl incarnate / lab rabbits included"
kids dont try anything annie does at home ,
for for scientific / educational review only.
 
nen888
#19 Posted : 2/10/2016 1:05:26 AM
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i've done the 'Hofmann' method once, with a friend...it works...as i mentioned in the thread i linked (i think) i would have done each wash twice, on reflection, to clean it up more..

i can't remember whether it was the chloroform or the acetone now, but one of those two pulled out this waxy stuff that at the time me and friend concluded was exactly the 'makes you nauseous' component..

the end result is smokeable, resulting in a rougly 45 minute experience


..i can't see how chloroform is any more of any issue, toxicity wise, than DCM


and no, like anne says...you don't want to mess with pH...it's not like other alkaloids in that way..
 
User_7
#20 Posted : 2/10/2016 10:17:16 PM

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I didn't realise that DCM was particularly toxic. From what I read about chloroform I was under the impression that it planned to saturate the air around me and knock me out before having its wicked way with my limp corpse. In any case DCM is much easier to acquire, do you think it would serve as a reasonable substitute? I already have acetone and naptha which I think I read someone used to clean psilocybin. Do you think it could be useful?

Then I was thinking more about something to store and dose it in. How about glycerine or propylene glycol? Anyone know if psilocybin is likely to dissolve in either and how it might affect shelf life? As well as being food safe I could then try vaping it :-)
 
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