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Offlineionic
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Registered: 06/03/01
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Actual Extractors, Psilocybin Crystals
    #591324 - 03/27/02 08:20 PM (22 years, 6 days ago)

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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Invisiblealtarego
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Registered: 10/25/01
Posts: 130
Re: Actual Extractors, Psilocybin Crystals [Re: ionic]
    #591390 - 03/27/02 09:38 PM (22 years, 6 days ago)

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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InvisibleSumGuy
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Registered: 07/26/01
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Re: Actual Extractors, Psilocybin Crystals [Re: ionic]
    #591633 - 03/28/02 06:10 AM (22 years, 5 days ago)

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.


--------------------
-SumGuy :cool:

Edited by SumGuy (03/28/02 06:11 AM)

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OfflinePeyotl
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Re: Actual Extractors, Psilocybin Crystals [Re: SumGuy]
    #591747 - 03/28/02 09:26 AM (22 years, 5 days ago)

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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InvisibleSumGuy
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Re: Actual Extractors, Psilocybin Crystals [Re: Peyotl]
    #591796 - 03/28/02 10:33 AM (22 years, 5 days ago)

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.


--------------------
-SumGuy :cool:

Edited by SumGuy (03/28/02 10:34 AM)

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OfflineAnnoA
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Re: Actual Extractors, Psilocybin Crystals [Re: ionic]
    #591840 - 03/28/02 11:41 AM (22 years, 5 days ago)

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 :wink:

Edited by Anno (03/28/02 11:48 AM)

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OfflineSeussA
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Re: Actual Extractors, Psilocybin Crystals [Re: Anno]
    #591903 - 03/28/02 01:06 PM (22 years, 5 days ago)

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.


--------------------
Just another spore in the wind.

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OfflineAnnoA
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Re: Actual Extractors, Psilocybin Crystals [Re: Seuss]
    #591943 - 03/28/02 02:01 PM (22 years, 5 days ago)

She would be removing water from the 96% ethanol by adding a hygroscoping salt, like calcium chlorid.

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InvisibleSumGuy
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Re: Actual Extractors, Psilocybin Crystals [Re: Anno]
    #592008 - 03/28/02 03:16 PM (22 years, 5 days ago)

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.


--------------------
-SumGuy :cool:

Edited by SumGuy (03/28/02 03:24 PM)

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OfflineAnnoA
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Re: Actual Extractors, Psilocybin Crystals [Re: SumGuy]
    #592057 - 03/28/02 04:11 PM (22 years, 5 days ago)

>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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Offlineinvi
journeyman
Registered: 08/19/03
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Last seen: 20 years, 5 months
Re: Actual Extractors, Psilocybin Crystals [Re: Anno]
    #1976166 - 10/03/03 12:16 PM (20 years, 5 months ago)

@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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InvisibleMrMaddHatter
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Re: Actual Extractors, Psilocybin Crystals [Re: invi]
    #1978271 - 10/04/03 02:00 AM (20 years, 5 months ago)

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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Offlineinvi
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Re: Actual Extractors, Psilocybin Crystals [Re: MrMaddHatter]
    #1978588 - 10/04/03 07:28 AM (20 years, 5 months ago)

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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InvisibleMrMaddHatter
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Re: Actual Extractors, Psilocybin Crystals [Re: invi]
    #1979260 - 10/04/03 03:08 PM (20 years, 5 months ago)

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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Offlineinvi
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Re: Actual Extractors, Psilocybin Crystals [Re: MrMaddHatter]
    #1981727 - 10/05/03 03:54 PM (20 years, 5 months ago)

how would you recrystalize ?

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InvisibleMrMaddHatter
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Re: Actual Extractors, Psilocybin Crystals [Re: invi]
    #1981793 - 10/05/03 04:36 PM (20 years, 5 months ago)

I didn't mean recrystallize..I was a little :pill2: :nut: :stoned: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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Invisiblechris_kelvin
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Re: Actual Extractors, Psilocybin Crystals [Re: MrMaddHatter]
    #1981925 - 10/05/03 05:43 PM (20 years, 5 months ago)

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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Offlineinvi
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Re: Actual Extractors, Psilocybin Crystals [Re: chris_kelvin]
    #1983246 - 10/06/03 06:11 AM (20 years, 5 months ago)

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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Invisiblemicro
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Re: Actual Extractors, Psilocybin Crystals [Re: invi]
    #1983294 - 10/06/03 07:16 AM (20 years, 5 months ago)

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 :frown:

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 :frown:

Have fun, kids!

--
Micro


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(Avatar is Maxxy, a character by Mizzyam, RIP)

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InvisibleMrMaddHatter
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Re: Actual Extractors, Psilocybin Crystals [Re: micro]
    #1984086 - 10/06/03 02:23 PM (20 years, 5 months ago)

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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