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psilocybin extraction/tincture tek

ragabr said:
benzyme said:
it isn't like psilocin, which has that unprotected hydroxy group; so it isn't degraded by light or air. you don't even need inert atmosphere to extract it.
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The first time SWIM attempted this, she acidified with citric acid, with the thoughts of having psilocin instead. Does this mean exposure to light has degraded the product, or is it unlikely the citric acid actually converted the psilocybin to psilocin?
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there seems to be a lot of unresolved questions regarding the treatment of psilocybin with acid, though the (pKa) data with respect to the phosphoryl group suggests that it may be subjected to different charge states without being removed. the acid treatment would likely require moderate heat for any conversion to occur; of course, this should be in inert atmosphere, and in some form of dim lighting (ex. red light)
 
nen888 said:
..here is a great old lycaeum thread for those interested in "Simple Psilocybin & Psilocin Extraction": http://forums.lycaeum.org/index.php?topic=26844.0..also, apparently the original Albert Hoffman psilocybin extraction tek produces a blue/grey 'crystal' which can be smoked to produce a 45 minute experience [Jim deKorne in his final issue as editor of E.R. - he had successfully done this, but was surprised others hadn't..]
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ps. anyone got the Hoffman '50s paper? i believe it used a chloroform wash, an acetone wash, and then extraction into basic methanol..
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I don't want to spread a rumor, so be informed that I am not 100% sure, but haven't the crystals from the first tek been reported to be almost pure sugar? I recall reading this somewhere..
 
benzyme said:
that's a rumor.
it's neither pure sugars, nor pure alkaloids..but likely a mixture of both.
ethanol and methanol are non-specific with respect to what they pull.
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Hm, but as sugar is afaik not soluble in dcm and acetone (at lest at room temp) it might be pretty hard to clean the mix.
 
So when it comes to the prefered solvent, I figure that methanol is the best way to go?
 
..i didn't know sugars dissolved in methanol either..
endlessness wrote:
Nen, what is the paper you are talking about?
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..the original Albert Hoffman psilocybin extraction formula to produce 'crystal' c.1950s
i'm pretty sure it went like this: dry/powder mushrooms, wash with acetone..dry, wash with chloroform..dry, extract with basic methanol and evaporate to almost pure mushroom alkaloids..i have done this once with a friend..the chloroform pulled a ball of waxy stuff that had the 'makes you want to puke' smell..it was decided the cleaning washes weren't complete enough as the final product was a dark oil..it worked vaporized!
 
..found the basic info. based on the Hoffman technique: (chloroform wash first)
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.
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This seems to be a relatively simple extraction per this method. I am curious as a more recent letter Alexander Shulgin posted he made no claims to this method, however he clearly stated that psilocybin extracted with is most soluble in water, and very inefficient with methanol & psilocin had most success with ethanol and quoted methanol as extremely inefficient. I have a strong understanding of science but no chemistry background but I only mention what Mr. Shulgin quoted as he is a very reputable source for the science of psychedelics :) Seems to me under his method you would want to look at 70% because it was most efficient for psilocin and contains water the most efficient solvent for a simple soak and base but I could be wrong? I know it's not very common to find but you can always look at adding distilled water to Everclear as a possible solution?

Next project is to do a soak or agitation in a jar by putting a few marbles, and mushroom material in a jar then run in a rock tumbler. Mr Shulgin also makes mention of the slower time associated with the extraction of the psilocin so how much time would be appropriate to maximize efficiency? Part 2 of the project would involve taking gummy bears and soaking in the ethanol solution until absorbed. Google vodka gummy bears it's a fun project even from the alcohol standpoint :)
 
That would be a question for Mr Shulgin as he stated that in his letter but can be quoted just as stated in the previous post. I couldn't find the original paper he quoted "citation to the article is Kysilka, R. and Wurst, M., Planta Med. Vol. 56 pp. 327-328 (1990)." I only found the intro to the paper and it states that in fact 75% methanol was most efficient for psilocybin and 75% ethanol/water for psilocin - different from the letter Mr Shulgin wrote :) I guess it should be figured out if the goal is to make the simplest efficient tincture or if the goal is the pure isolation of psilocibin or psilocin?

P.S. Thanks for your time Benzyme, it eliminates a lot of guesswork when a skilled chemist is involved.
 
Suggested experiment:


Finely chop up some shrooms. Do the ethanol soak, collect the the crystals and vaporize them. I expect failure to launch off into hyperspace via this method--the tek has been around around for awhile, yet the concept of smoking it still exists as a rumour and a legend.


But, has anyone taken this mushroom sugar/psilocybin/psilocin crystal, added some harmalas and vaped that?
 
Bedazzle said:
Finely chop up some shrooms. Do the ethanol soak, collect the the crystals and vaporize them.
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calling them crystals is a stretch. "crystals" imply a fairly pure product, and an alcoholic extraction is far from it. it's a precipitated mixture of alkaloids and proteins, which is why once the alcohol evaporates, the product has a greenish color.
 
jamie said:
nen888 said:
it worked vaporized!
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it worked? Can you elaborate?
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..in his final editorial of E.R. in 1998 (i will post the actual text when i can find it) Jim de Korne said that he had tried the Albert Hoffman technique for psilocybin extraction (i posted this earlier in thread) and had produced a 'blue-grey crystal' which, vaporized, led to a 45 minute psilocin experience similar to a milder smoked DMT experience, but with it's own character (sounds a bit like DET)..it was probably not actually pure crystal, but sounds quite refined - compared to the dark brown gunk i got, the one rushed attempt i had at this method - this still had activity smoked, but was only enough for the mildest of visuals..it showed promise..it was like mushrooms smoked :)

He had written up this info in the journal before, and was surprised that no one else had reported trying it..i have been planning to try this properly one day..
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..to elaborate further..
i am trying to access all the original De Korne references, as i have a feeling he may have converted to the base..the mild dark brown gunk i tried was not the base..this, plus better purification should make a difference..

..when i first read De Korne's statement 14 years ago it immediately struck me that there was no logical reason why freebase psilocybin/psilocin would not be active, and as potent as oral ingestion..it made sense that the duration was shortned..the onset was not as fast as DMT..


..so, the next time i see a big shroom fruiting season (which probably won't be for a while) i will adapt the 'Hoffman Proceedure' as follows:
1. Dry the mushrooms within 24-48 hours.
2. Crush the dried carpophores to a powder.
3. Add twice volume of chloroform (or other halogenated hydrocarbon non polar solvent).
Shake vigorously and allow to stand for 2-4 hours.
4. Filter and discard the chloroform.
5. Add chloroform as step 3, shake, stand for 30 minutes.
6. Filter and discard the chloroform.
7. Add twice volume of acetone, shake and stand for 1-2 hours.
8. Filter and discard the acetone. Probably repeat this step one more time.
9. Add 150% volume methanol, shake and allow to stand 4-8 hours. Filter, keep methanol.
10.Add methanol, repeat step 9, stand for less time. Filter, keep methanol.
11.Repeat methanol step third time. Discard residue.
12.Combine methanol extracts.
...at this point i am improvising..
13.Add NaOH+very small amount H20, or other basifying agent, until methanol somewhere between ph 9-12.
14.Evaporate methanol to dryness, preferably in a vacuum, or low heat will do.
15.Recrystalize solid from methanol. Store cold, away from air, light, moisture.
..vaporize 10-30mg in glass chamber..

any suggested improvements? can't wait to try it again, in this fashion..
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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.
You guys rock!!! :D
You can do it!!!
 
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