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 ionic
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 Actual Extractors, Psilocybin Crystals 
#591324 - 03/27/02 08:20 PM (21 years, 8 months ago) |
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When it comes to the real basic chem that we talk about here, there is a great amount of theory and very little actual experimentation.
I am one of these, unfortunately. I read through the PFTek extraction and was curious. The ethyl alcohol is a polar solvent, so all the polar salts will come into solution, whatever form psilocybin is in the mushroom. When someone makes tea they add a little acid to salt whatever possible freebase psb is in the pulverized shroom. I was curious about someone who may have tried to get freebase PSB to precipitate by adding some sort of base (I would use pure lye.) Once this is done streaks of freebase psb should precipitate from solution and settle to the bottom of the glass. The gross solution could be removed by simply pouring off and evaporating. Could this product be used in any way and how. It would be fun to put this into some non-polar solvent (I've been leaning towards DMSO) to dissolve this freebase and then salt it again using another acid.
Anyone who has tried any form of extraction, please give us a little experience.
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 altarego
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 Re: Actual Extractors, Psilocybin Crystals [Re: ionic]
#591390 - 03/27/02 09:38 PM (21 years, 8 months ago) |
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Ok -
This is written from extensive chemistry experience, and EXTREMELY limited (read: no) experience with psilocybin/psilocin purification.
Allow me to explain:
Psilocybin and psilocin are what is known as a zwittwerion, German for "self-salt", meaning it has a basic (the "amino" in tryptAMINE) end, and an acidic portion (the phosphate, or hydroxyl bit), which "neutralize" each other, in a crude sense, meaning that a) psilocybin/psilocin are salts, therefore readily soluble in H20, and 2) there is no such thing as "freebase" psilocybin or psilocin. You might however be able to make another salt form of them by using a strong acid, such as HCl.
If you wanted pure psilocybin/psilocin you would want to avoid aqueous extractions (their ready solubility would make them difficult to extract), and instead find a suitable organic solvent from which to recrystallize them. (There is literature on this.)
Why anyone would need to do this, beats me, since there is nothing you can do with pure compounds that you can't get from tea or eating.
- AE
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SumGuy
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Re: Actual Extractors, Psilocybin Crystals [Re: ionic]
#591633 - 03/28/02 06:10 AM (21 years, 8 months ago) |
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Well when you grind your mushrooms and soak in pure methanol for a good 5 days, filter, and evaporate it by natural evaporation in a dust free environment over a period of about a week you'll have a very very potent sticky residue. Thus being said since you wouldn't want the sticky residue, which I would immagine is just natural sugars/waxes or whatever happens to be in mushrooms, you could try soaking in chloroform for a few days, filter, then discard your chloroform, then keep your mushroom dust left in the filter and then try a methanol extraction. My guess is that you would be left with a pretty pure extraction because the chlorofrom would only extract the residue. Since chloroform is hard to aquire you could always TRY a non-polar solvent like naphta (which is very easy to aquire) in place of chloroform, I'm not sure which would be better to use really but I believe chloroform is the best choice to remove those waxes etc..
I have zero experience with this and I dont recommend doing this as this is an exteremely strong alkaloid that is not only illigal but should not be used by an amatur without a very accurate scale for measuring doses.
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-SumGuy 
Edited by SumGuy (03/28/02 06:11 AM)
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Peyotl
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Re: Actual Extractors, Psilocybin Crystals [Re: SumGuy]
#591747 - 03/28/02 09:26 AM (21 years, 8 months ago) |
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dont know how smart it is to run a bunch of other chens through your body like this. i wouldnt do it.
that being said, wouldnt it be easier to increase the acidity of water? like by squeezing some jalepeno [sp?] in it? doen sound as crazy as drinking rubbing alcohol. i could be way off base tho.
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SumGuy
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Re: Actual Extractors, Psilocybin Crystals [Re: Peyotl]
#591796 - 03/28/02 10:33 AM (21 years, 8 months ago) |
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You dont actually ingest these chemicals, they are filtered off or evaporated. This is just a basic extraction in pretty much the same way many essential oils are extracted from plants.
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-SumGuy
Edited by SumGuy (03/28/02 10:34 AM)
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Anno
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Re: Actual Extractors, Psilocybin Crystals [Re: ionic]
#591840 - 03/28/02 11:41 AM (21 years, 8 months ago) |
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A friends grandmother took a different approach:
She told him she extracted fine mushroom powder with hot water for only a few minutes,filtered through a fine filter, discarded the mushroom powder and evaporated the extract by boiling.
Then she poured the thick syrup on a plate and let the rest of the water evaporate by pointing a fan on it.
This left a brownish hard residue on the plate (she told him it looked and feeld like caramel) which she scraped off with a knive.
This is a picture she made of the resulting powder:
Now she wondered, and I wasn?t able to give her a definitive answer:
Could she dissolve this powder in pure (100% !! ) ethanol and obtain pure psilocybin this way?
She told me, that according to the MERCK manual ( http://www.erowid.org/plants/mushrooms/mushrooms_chemistry.shtml ), psilocybin is nearly insoluble in pure ethanol, thus should remain in chrystal form at the bottom of the extraction flask....
I don?t know, does anyone?
PS: When I asked her why she bothered extracting it at all, she said she was bored 
Edited by Anno (03/28/02 11:48 AM)
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Seuss
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Re: Actual Extractors, Psilocybin Crystals [Re: Anno]
#591903 - 03/28/02 01:06 PM (21 years, 8 months ago) |
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You will have to distill your ethanol before hand or the excess water in the ethanol will suck up your goods. You will probably also loose most of your psilocin into the ethanol if I remember correctly. I think chloroform would probably be a much better choice.
If you really want to isolate the psilos, I would look into liquid chromatography.
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Just another spore in the wind.
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Anno
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Re: Actual Extractors, Psilocybin Crystals [Re: Seuss]
#591943 - 03/28/02 02:01 PM (21 years, 8 months ago) |
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She would be removing water from the 96% ethanol by adding a hygroscoping salt, like calcium chlorid.
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SumGuy
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Re: Actual Extractors, Psilocybin Crystals [Re: Anno]
#592008 - 03/28/02 03:16 PM (21 years, 8 months ago) |
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Anno she could also use anhydrous MgSO4 (epsom salts) to make the ethanol anhydrous. By extracting with water aren't you missing out on the psilocin? Perhaps after doing a chloroform extraction to remove the things that made the caramel texture you would yeild both the psilocin and psilocybin by using the ethanol w/ the 4% water in it.
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-SumGuy
Edited by SumGuy (03/28/02 03:24 PM)
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Anno
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Re: Actual Extractors, Psilocybin Crystals [Re: SumGuy]
#592057 - 03/28/02 04:11 PM (21 years, 8 months ago) |
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>By extracting with water aren't you missing out on the psilocin?
She is, but psilocin is a minor component which is also very unstable, so she would be happy with mostly psilocybin, she said.
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invi
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Re: Actual Extractors, Psilocybin Crystals [Re: Anno]
#1976166 - 10/03/03 12:16 PM (20 years, 2 months ago) |
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@ANNO :
how does this came out in the end ?
How much gramms of Calcium Carbonat are needed per Liter of 96% Ethanol ?
Do you think you got a bit percentage of the psilocybin in the fruitbodies to crystalize ?
i would like to extract the magic crystal,
so does anyone has a working TEK ?
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MrMaddHatter
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Re: Actual Extractors, Psilocybin Crystals [Re: invi]
#1978271 - 10/04/03 02:00 AM (20 years, 2 months ago) |
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Wow this is old. Just a quick thought. Methanol would have probably extracted the psilocybin from the brown powder in Anno's pic. As psilocybin is readily soluble in methanol.
Hmmm....this gives me an idea.
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invi
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Re: Actual Extractors, Psilocybin Crystals [Re: MrMaddHatter]
#1978588 - 10/04/03 07:28 AM (20 years, 2 months ago) |
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yes, methanol would have extracted it i guess;
but i think anno thought of doing it with ethanol,
cause it should form crystals, while with methanol it will be in the liquid and has to be evaporated, etc, ...
Quote:
according to the MERCK manual ( http://www.erowid.org/plants/mushrooms/mushrooms_chemistry.shtml ), psilocybin is nearly insoluble in pure ethanol, thus should remain in chrystal form at the bottom of the extraction flask...
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MrMaddHatter
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Re: Actual Extractors, Psilocybin Crystals [Re: invi]
#1979260 - 10/04/03 03:08 PM (20 years, 2 months ago) |
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Ethanol could be used to wash out the impurities I suppose. Though personally I would rather dissolve in methanol and recrystalize.
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invi
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Re: Actual Extractors, Psilocybin Crystals [Re: MrMaddHatter]
#1981727 - 10/05/03 03:54 PM (20 years, 2 months ago) |
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how would you recrystalize ?
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MrMaddHatter
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Re: Actual Extractors, Psilocybin Crystals [Re: invi]
#1981793 - 10/05/03 04:36 PM (20 years, 2 months ago) |
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I didn't mean recrystallize..I was a little    last night. What I meant was dissolve in methanol and precipitate the crystals by evaporating the psilo/methanol solution to half the original volume then sticking in freezer to precipitate crystals. Slow evap or somethin.
Thats all theory though. Have no idea if it'll work.
Edit:: The Hive would probably be a better place to discuss these matters.
Edited by MrMaddHatter (10/05/03 04:37 PM)
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chris_kelvin
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 Re: Actual Extractors, Psilocybin Crystals [Re: MrMaddHatter]
#1981925 - 10/05/03 05:43 PM (20 years, 2 months ago) |
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I wouldn't be afraid of the 4% water making much difference at all because in Merck Index they say that psilocybin (the zwitterionic form that is) can be recrystallized from boiling water, and that one gram dissolves in 20 grams of boiling water or 120 grams of boiling methanol. It's solubility is much much lower (one could say it is sparingly soluble, if not insoluble) in cold water or methanol, so the 96% ethanol is quite ok.:)
How to recrystallize? Ideally, if you wanted to recrystallize one gram of psilocybin, you would dissolve dissolve the stuff in 20 grams (or a bit more) of boiling water or 120 grams of boiling methanol (methanol is toxic, but I guess you knew that already) and let it cool down slowly. The psilocybin would then hopefully crystallize, as its solubility is lower in a cold solvent. The tricky part is that you might have some stuff there that won't dissolve at all, and you would have to filter it hot, and even after that you might have stuff there that would also crystallize when the solvent cools down, if it wouldn't make the whole crystallization impossible. A lot of unknowns.
Of course, chromatography is the way professionals do it, but it's tedious.
A note on drying ethanol: Distilling the 96% ethanol doesn't help because it is the same stuff that distills over. There are few drying agents that can be used to make absolute ethanol. Calcium chloride, calcium carbonate or MgSO4 won't stand a chance.
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invi
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Re: Actual Extractors, Psilocybin Crystals [Re: chris_kelvin]
#1983246 - 10/06/03 06:11 AM (20 years, 2 months ago) |
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thats just the way i wanted to do it,
but when i wanted to figure out the right amounts i saw it will not be possible to extraxt and crystalize with only water.
i guess the problem with 20 parts/120parts water
will be the following :
1 gramm cub is around 5-10mg psilocybin.
20 x 10mg = 200mg
200mg Water = 0,2 ml Water
(cause : 1 Liter Water = 1kg; 1 Gramm water = 1 ml Water)
so how to add just 0,2ml water per gramm of cubs and still get something like a liquid ?
@MrMaddHatter
i have a problem with the hive : cannot search anything,
cause it everytimes wants to open the secure sites, but my proxy does not support that.....
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micro
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Re: Actual Extractors, Psilocybin Crystals [Re: invi]
#1983294 - 10/06/03 07:16 AM (20 years, 2 months ago) |
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Altarego -- psilocybin is not readily water-soluble; it will only dissolve if heated. It's soluble only in *acidic* polar solutions (and basified nonpolar solutions.) It's not a salt by itself -- it would be considered a freebase.
Anno -- psilocybin should be ethanol soluble. I wouldn't do an ethanol wash -- cold water if anything, but for polar/nonpolar extractions you'll have to pH 
Mr. Mad Hatter (do I know you?) -- You recrystalize by making the chemical insoluble -- easiest way in this case would probably be to add lots of distilled water and chill it, but I have no clue off the top of my head how soluble it would be in a dilute alcohol solution. Without this you might not get anything. I've only evaporated it -- never found a way to get a precipitate, sorry
Have fun, kids!
--
Micro
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MrMaddHatter
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Re: Actual Extractors, Psilocybin Crystals [Re: micro]
#1984086 - 10/06/03 02:23 PM (20 years, 2 months ago) |
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Quote:
micro said:
Mr. Mad Hatter (do I know you?)
I don't know. Possibly, but I doubt it. What makes you ask?
Have you tried chilling a methanol solution to preciptate. I don't think I've ever heard of anyone doing it.
@Invi--You'll have to drop the proxy to search the hive. I wouldn't worry about IP security there as long as your not posting.
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PNutButta
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Re: Actual Extractors, Psilocybin Crystals [Re: MrMaddHatter]
#1984193 - 10/06/03 03:08 PM (20 years, 2 months ago) |
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Adding small amounts of HCl, one drop at a time to a Methanol solution will cause precipitation.
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MrMaddHatter
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Re: Actual Extractors, Psilocybin Crystals [Re: micro]
#1984466 - 10/06/03 05:02 PM (20 years, 2 months ago) |
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I've been researching and come to the conclusion that psilocybin is not affected by heat(not too much heat anyway). So a boiling water bath to evap in wouldn't harm the psilocybin just the psilocin, correct 
A friend of mine left a hot water extract to evap in a steaming hot water bath and accidentally fell asleep and everything evaped even the water in the bath. Don't know how long this set like this (maybe 2-4hrs.) Will this degrade the psilocybin? Psilocybin has a melting point of 220-228? C. The temp was well below that.
@PNutButta--Sounds feasible
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micro
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Re: Actual Extractors, Psilocybin Crystals [Re: MrMaddHatter]
#1984657 - 10/06/03 06:08 PM (20 years, 2 months ago) |
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MH -- it shouldn't break the psilocybin down right away, but enzymes can. Don't know details, but I'd eat it right away
PNutButta -- any references? Have you done this yourself? It doesn't really make sense to me -- psilocybin seems to dissolve in protic solvents when acidified -- why would adding HCL make it precipitate out of an alcohol?
Just curious.
--
Micro
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invi
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Re: Actual Extractors, Psilocybin Crystals [Re: micro]
#1984787 - 10/06/03 07:00 PM (20 years, 2 months ago) |
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when buying hcl,
which concentration is good ?
i heard the solution should be brought to ph 3,
so how much hcl of which concentration is approximately needed on 10 ml solution ?
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invi
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Re: Actual Extractors, Psilocybin Crystals [Re: invi]
#1984847 - 10/06/03 07:29 PM (20 years, 2 months ago) |
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the denaturated ethanol i can get ist denaturated with "Methylethylketon"...can i safely use it ?
i think so, cause i read up in the net that it is a solvent that will easily evaporate at roomtemp.
i hope without any leftover...
anyone knows better ?
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micro
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Re: Actual Extractors, Psilocybin Crystals [Re: invi]
#1984857 - 10/06/03 07:34 PM (20 years, 2 months ago) |
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How many drops do you want to add before something will happen?
--
Micro
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micro
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Re: Actual Extractors, Psilocybin Crystals [Re: micro]
#1984883 - 10/06/03 07:45 PM (20 years, 2 months ago) |
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Invi -- denatured ethanol just has 5% methanol/isopropanol in it. It will safely evaporate and leave your product, but don't ingest any of the alcohol. Once it evaporates it's gone -- just make sure you smell no alcohol after it's dry.
--
Micro
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Any research paper or book for free
(Avatar is Maxxy, a character by Mizzyam, RIP)
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invi
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Re: Actual Extractors, Psilocybin Crystals [Re: micro]
#1984948 - 10/06/03 08:12 PM (20 years, 2 months ago) |
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i do not understand, what you are really asking for;
think is my english
i found a recipe, which sounds good to me on the net,
and wanted to know how much HCL i should use :
Quote:
1. Powder mushrooms in blender
2. soak powder in 140 proof ethanol = 70 percent alcohol. Soak for 12 hours (or so), in the fridge but
roomtemp is probably OK too.
2a)Then pour the liquid through an old white t-shirt or so in a 2nd jar. Fill a syringe with it,
attach a filter and empty the syringe in jar no. 3
The filtration can be done with a disposable 0.2 micrometer liquid filter for
syringes (handpowdered, so no electricity or adspirator is needed) because you do not need to
save the insoluble particles. The filter can be discarded.
3. evaporate the liquid (big shallow dish, table fan) to 1/10 of the volume
(until it has just not begun to crystallize out)
4. add a few drops of hydrochloric or muriatic acid to convert all ionic and freebase alkaloids into salts
5. put the acidified extract in a tall vial
6a. remove resins with naphta or petroleum ether. These liquids float on top of the extract. To remove the
resins, just add naphta or pet ether, shake, let settle and remove/separate the layers with a pipette or
syringe. Discard the naphta/pet ether.
6b. repeat step 6a.
7. Now add acetone and repeat step 6a+6b.
7a) wash with 95 percent alcohol (cold)
The dark granular stuff which remains is a mixture of alkaloids. Among those are the alkaloids you want.
8. Add 190 proof or 95-96 percent ethanol (denatured alcohol is no problem as long it is denatured with
methanol or acetone). Close the vial and place it in boiling water. If you have a small,
thick walled glass bottle or vial you can even place it in a pc.
9. Wait until the vial is of the same temperature, take it out of the water and allow it to
cool down to slightly below the boiling point of the ethanol (so you can safely open the lid)
Suck up the liquid in a syringe, filter it and allow it to cool down slowly.
9a) The fine white crystals which precipitate
(rain down) as first from the solutiuon is what you are looking for.
White psilly crystals precipitate, urea stays in solution
(as long as you don't evaporate the liquid too far of course).
10. Remove the excess liquid with a pipette or syringe. Save the crystals.
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MrMaddHatter
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Re: Actual Extractors, Psilocybin Crystals [Re: micro]
#1985114 - 10/06/03 09:01 PM (20 years, 2 months ago) |
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Thanks for the info Micro. Could you explain more on the enzymes breaking down psilocybin or provide some links.
Quote:
micro said:psilocybin seems to dissolve in protic solvents when acidified -- why would adding HCL make it precipitate out of an alcohol?
Very good point.
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invi
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Re: Actual Extractors, Psilocybin Crystals [Re: MrMaddHatter]
#1986618 - 10/07/03 11:26 AM (20 years, 2 months ago) |
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i am in search for naptha or petroleum ether.
Actually i am living in germany, i know i can get the stuff from a pharmacie, but i found 2 things much cheaper :
1)turpentine replacement
its mostly (solvent)naptha but also with "paraff. , aliphatic and aromatic hydrocarbons"
paraff. is for sure paraffins...
2)brush cleaner
also mostly (solvent)naptha but with "nonionic tensides"
i think the first one should evaporate without any leftover, the second will leave over some tensides after evaporating....
am i right ?
anyone knows ?
cause i dont want to have some chemicals of the solvents left in my "endproduct"...
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MrMaddHatter
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Re: Actual Extractors, Psilocybin Crystals [Re: invi]
#1987066 - 10/07/03 02:24 PM (20 years, 2 months ago) |
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I wouldn't trust anything that has additives. You want your solvents absolutely clean.
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cricket
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Re: Actual Extractors, Psilocybin Crystals [Re: MrMaddHatter]
#1987075 - 10/07/03 02:27 PM (20 years, 2 months ago) |
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Zippo lighter fluid is usualy made from Naptha.
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I tried to leave my signature but it didn't work...
By the way... Does anybody know how to get sharpie markers off of a computer screen?
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invi
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Re: Actual Extractors, Psilocybin Crystals [Re: cricket]
#1987325 - 10/07/03 03:49 PM (20 years, 2 months ago) |
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i think as long as all the additives will evaporate like the solvent there should be no problem - no one wants to drink/smoke/... naptha; but we dont have a fear cause everything of it evaporates.....
the problem with lighter/zippo fluid : i did not find one package with a real list of ingridients....
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micro
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Re: Actual Extractors, Psilocybin Crystals [Re: invi]
#1989437 - 10/08/03 07:44 AM (20 years, 2 months ago) |
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Invi -- Get some muriatic acid from a home supply store (a lot of times in the gardening center) -- this is concentrated HCl.
MH --
"The occurence and extraction of indole derivatives in six species from four genera of higher fungi were investigated. By using pure methanol concentrations of psilocybin and baeocystin. The psilocin content of the species was higher by using aqueous solutions of alcohols than with methanol alone but was an artificial phenomenon caused by enzymatic destruction of psilocybin."
http://www.erowid.org/plants/mushrooms/mushrooms_journal1.shtml
Hot water will extract a lot of enzymes (dephospholrylases?) which could convert psilocybin -> psilocin (unstable.) Heating also makes the enzymes work faster, up to what point I don't know (they should just stop and start to denature at some temp.)
Making tea obviously works, though, so the psilocybin can last a while. Over a matter of hours, though, I don't know -- if it wasn't boiling it might be o.k.
--
Micro
--------------------
Any research paper or book for free
(Avatar is Maxxy, a character by Mizzyam, RIP)
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MrMaddHatter
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Re: Actual Extractors, Psilocybin Crystals [Re: micro]
#1989491 - 10/08/03 08:33 AM (20 years, 2 months ago) |
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Thanks for the info 
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Infrared
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Re: Actual Extractors, Psilocybin Crystals [Re: invi]
#1989721 - 10/08/03 10:38 AM (20 years, 2 months ago) |
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naptha is crap, i wouldnt use it for anything that you plan on consuming. denatured ethanol or straight methanol is the best for a 4-ho-dmt extraction. toulene would be good if you wanted to recrystalize your final product.
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When chemistry is outlawed.. Only outlaws have chemistry
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invi
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Re: Actual Extractors, Psilocybin Crystals [Re: Infrared]
#1989882 - 10/08/03 11:41 AM (20 years, 2 months ago) |
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its not really for extraction...
its for washing the extract....
the naptha and everything in it will be disposed...
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MrMaddHatter
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Re: Actual Extractors, Psilocybin Crystals [Re: micro]
#1990157 - 10/08/03 01:22 PM (20 years, 2 months ago) |
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Micro, you said you've never got any to precipitate. What about PF's infamous chilled ethanol crystals? Have you tried this. You seem to know more about this kind of stuff than me, so, is PF's method even feasible?
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micro
bunbun has a gungun
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Re: Actual Extractors, Psilocybin Crystals [Re: MrMaddHatter]
#1990318 - 10/08/03 02:13 PM (20 years, 2 months ago) |
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I think he said to evaporate it, too. I don't think it would be efficient to just precipitate and filter because you'll prolly still have a lot left in the solution; depends on the Ksp but it's not only soluble in hot ethanol so I would think you'll lose a lot in solution. It would have to be toyed with, though -- I've never tried chilling the alcohol, just evaporating it.
Ethanol won't yield a pure product, anyway, so it wouldn't really be much different than just filtering and evaporating it, which works fine. If you want a pure product you have to extract it further than just alcohol.
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Micro
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MrMaddHatter
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Re: Actual Extractors, Psilocybin Crystals [Re: micro]
#1990495 - 10/08/03 03:27 PM (20 years, 2 months ago) |
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Gotcha. Do you or anyone know if this brown gunk left behind from extractions will stick to parchment paper? Stuffs hard to work with.
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micro
bunbun has a gungun
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Re: Actual Extractors, Psilocybin Crystals [Re: MrMaddHatter]
#1990632 - 10/08/03 04:21 PM (20 years, 2 months ago) |
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Probably. It does a pretty good job sticking to glass.... I always had to scrape it off with a razor blade. Why parchment paper?
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Micro
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MrMaddHatter
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Re: Actual Extractors, Psilocybin Crystals [Re: micro]
#1990676 - 10/08/03 04:33 PM (20 years, 2 months ago) |
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I saw someone had some honey oil on parchment paper and it wasn't sticking to it(on overgrow), and you know how honey oil is. I just needed some way to work with it after I got it scraped so I could weigh it and stuff . Maybe I should let it dry more.
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MrMaddHatter
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Re: Actual Extractors, Psilocybin Crystals [Re: MrMaddHatter]
#1991562 - 10/08/03 10:07 PM (20 years, 2 months ago) |
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Yea, parchment paper works pretty good.
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trade_om
An Old Omelette
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Re: Actual Extractors, Psilocybin Crystals [Re: ionic]
#2716812 - 05/22/04 10:20 PM (19 years, 6 months ago) |
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OK here's a quote from the Ask Dr. Shulgin site. Dont know if any of you guys know it, but it appears its alot easier to isolate pure compounds from the msuhrooms then you thought -
"Psilocybe Mushroom Extractions
Dear Dr. Shulgin:
A friend of mine performed a Soxhlet extraction of 12 grams of powdered Psilocybe cubensis, using 95% ethanol. When the 60 mL of extract cooled to room temperature, many small transparent, colorless crystals had formed on the bottom of the container and did not redissolve on agitation. Do you know what these crystals are? -- Journeyman
Dear Journeyman:
There is a fascinating report in the literature that gives a quantitative measurement of the efficiency of extraction of both psilocybin and psilocin from the mushroom Psilocybe bohemica. The citation to the article is Kysilka, R. and Wurst, M., Planta Med. Vol. 56 pp. 327-328 (1990). These Czechoslovakian scientists studied the efficiency of both methanol and ethanol as solvents, each containing varying amounts of water. The results were, to me, both unexpected and most provocative.
The isolation of psilocybin seemed to be quite reasonable. This alkaloid is reasonably soluble in boiling water from which it can be nicely crystallized. It is less soluble in boiling methanol, and almost insoluble in boiling ethanol. And the extraction efficiency is optimum with methanol and almost as good with ethanol. With both, the less water present, the better. The compound is, after all, a perfect example of a zwitterion, the internal salt of a phosphoric acid and an amine base.
But the numbers with psilocin are strange. With aqueous ethanol, the optimum extraction was with a 70% ethanol concentration, and the extraction efficiency dropped almost to zero when there was no water present. But methanol was extremely inefficient regardless of the amount of water present in it. These researchers were apparently surprised by these findings, as they explored further and uncovered other clues. Time is a factor. Psilocin is extracted at a much slower rate than is psilocybin because it is contained intracellularly in the plant, and thus slower to be gotten out. They conclude that many of the low psilocin assays of mushrooms are due to this difficulty of getting the alkaloid out of the plant and into the extracting solvent. Using this information they determined that the levels of psilocybin and psilocin are substantially the same in Psilocybe bohemica, in conflict with the published literature values where very small amounts of psilocin were observed.
Efficient extraction apparently requires patience.
As to the identity of the crystals that were drifting around in the cooled Soxhlet receiver, from their being insoluble in ethanol, and white, and transparent, I would guess that you are seeing pure psilocybin.
-- Dr. Shulgin"
Here is the link - http://www.cognitiveliberty.org/shulgin/adsarchive/extraction.htm
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YesItsMe
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Re: Actual Extractors, Psilocybin Crystals [Re: trade_om]
#2717561 - 05/23/04 05:40 AM (19 years, 6 months ago) |
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**From The Hive , posted by Yachaj**
"" Further simplification:
1) instead of MeOH take 140 proof EtOH (70 percent EtOH, 30 percent water). The advantage of this liquid is that it extracts both PSOH and PSOP at low temperatures, in 12hrs time, but it is not as toxic as MeOH and more commonly available.
2a) evaporate it down until everything is just liquid. Add plenty of 190+ proof EtOH and a few drops of HCl. PSOP precipitates out!
2b) you can also evaporate all the 140 proof. The end result is a piece of brown gunk. This piece can be placed in 190+ proof EtOH (+ a drop of HCl). Don't touch it, just watch. In a few days to a week, lots of white dust separates from the brown gunk and collects on the bottom of the container.
Correct me if I am wrong but my explanation of the phenomenon is as follows. Compare it to a bottle of NaCl saturated water, which is visible because of the thin layer of table salt on the bottom. It looks as if the salt doesn't dissolve because the water has dissolved all the NaCl it can hold. But in reality the salt is constantly dissolving and precipitating at the same speed. So the layer stays the same.
Now compare this to a brown gunk of urea/psop with impurities in a bottle of 190+ proof EtOH with HCl.
Slowly the brown gunk dissolves, releasing both urea and PSOP. Urea stays in solution but the solvent is saturated with PSOP HCl in no time. It precipitates out!
But nevertheless, more PSOP HCl is dissolving from the brown gunk. And precipitates out. The chance for an individual PSOP HCl particle to precipitate back into the brown gunk is much smaller compared to the chance of precipitating on the bottom of the container.
Even more funny: the solvent is saturated with PSOP HCl. That means that, if you know the quantity of PSOP HCl which is dissolved in this solvent, at this pH and temperature, (in mg/ml), then you know exactly how many ml are needed for a dose. And this is totally independent from the potency of the mushrooms. Just prepare the PSOP in EtOH&HCl mixture and you know how many ml are needed.
No chromatography. No scales (except for the 1st time to determine the solubility data). No weird solvents, no rocket science - just vodka (separated into its constituents, EtOH and dihydrogen monoxide). Fat chance that the HCl isn't even needed. ""
Original Thread
Now other thing :
If u prepare tea with mushrooms ,let to room temp then place the extract in a ice bath , some white stuff precipitate .Rewash crystals with acetone to discard impurities .
But the yield is quite bad .
In this 2 techniks , u will extract psilocybin but not ( or really less) psilocin .
Psilocybin is quite stable compare to psilocin but only active orally .
So some guys prefer to extract psilocin , so they should follow this tek .
"Rhodium dephosphorilate psilocybin to psilocin with acetic acid "
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God  save the Queen
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micro
bunbun has a gungun
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Re: Actual Extractors, Psilocybin Crystals [Re: trade_om]
#2719887 - 05/23/04 07:11 PM (19 years, 6 months ago) |
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This has been discussed many times. The reason Shulgin came up with the results of psilocybin solubility in aqueous alcohol solutions is because of the enzymatic dephosphorylation of psilocybin.
--
Micro
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Alkaloids
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Re: Actual Extractors, Psilocybin Crystals [Re: micro]
#2806396 - 06/18/04 03:53 PM (19 years, 5 months ago) |
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Actually boiling water should completely denature the enzymes responsible for the dephosphorylation at temperatures well below the boiling point of water. Unless there are some unusual heat shock proteins in Psyilocybe sp. then you won't have to worry about further enzymatic conversion. If in doubt the mushrooms (whole or powdered) can be dropped into already boiling water which will heat kill the enzymes within a very short time period.
Sometime this summer I will see if my fuzzy friends can do some reasonably efficient extractions with various H2O and EtOH solutions. Might be able to check the results with GC/MS, but that will depend on availability at the time.
If the recrystallization is done in a glass container, reasonably pure, and dry then there should not be any difficulties removing the crystals using a small steel spatula/spoon.
good luck everybody
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micro
bunbun has a gungun
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Re: Actual Extractors, Psilocybin Crystals [Re: Alkaloids]
#2806425 - 06/18/04 04:04 PM (19 years, 5 months ago) |
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If you are using boiling water why not just do an A/B extract? You can't expect to recrystallize without first doing an appropriate extraction -- there are far too many compounds in mushrooms soluble in boiling water or alcohol or both.
The "enzymatic degredation" had to do soley with some experiment Shulgin did that said psilocin was more soluble in aqueous solutions of alcohol (enzymes are usually inactive in anhydrous alcohol.) They should both (phosphorylated or not) be really alcohol soluble -- that's all.
Boiling water should denature enzymes -- I agree, but without water enzymes aren't really active, anyway, and they should be extraced out with water in an acid/base extraction.
--
Micro
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(Avatar is Maxxy, a character by Mizzyam, RIP)
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Alkaloids
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Posts: 743
Loc: pubis mons
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 Re: Actual Extractors, Psilocybin Crystals [Re: micro]
#2944414 - 07/30/04 11:47 AM (19 years, 4 months ago) |
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Excellent points. Next time I'll try not to post when I am that tired.
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