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Invisibleblahblahblah
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Registered: 10/25/01
Posts: 1,022
Loc: South America
Re: all you need to know about psilocybin / psilocin extraction. [Re: UnderNose]
    #9650695 - 01/21/09 10:19 AM (13 years, 1 day ago)

I think the monotub has made this a better time for everyone to experiment with this. Good casings for me used to yield an ounce, now with the monotub, they yield a 1/2 pound. That is a lot of mushrooms to just have laying around. Seems that most of us here aren't in this to produce bulk and sell... maybe more people will start experimenting with extraction methods. If you could grow for a few months and condense it down, you could produce a years worth of mushrooms and keep the extract in your freezer without having to expain what the trashbag in the deep freeze is.

So to update (1-21 pics), the 70%'s top layer is black today. The fan was a very bad idea. It didn't effect the 92% at all, which would suggest that most of what was extracted in the 92% was Psilocybin. I might try and pick up some ascorbic acid fizzy tabs. The local health food store sells those, but not pure ascorbic acid (mine is being shipped later this week, won't be here for 10+ days). I think fastfred said earlier in this thread that they would work, he just wouldn't prefer it because of the sugar in them? I was kind of hoping he would chime in. He seemed pretty amped on these experiments previously.

One other note, I realized that I have calcium hydroxide... see this thread http://www.shroomery.org/forums/showflat.php/Cat/0/Number/4338772/page/0/fpart/1/vc/1 Maybe I should try the jungle extraction soon.


Edited by blahblahblah (01/21/09 01:21 PM)


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Invisibleblahblahblah
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Re: all you need to know about psilocybin / psilocin extraction. [Re: blahblahblah]
    #9651479 - 01/21/09 01:14 PM (13 years, 1 day ago)

So I tested the ascorbic acid fizzy tablets. I added 1 tablet to 100ml of water and then waited for it to stop fizzing. I took 20ml of the blue extract and added 5ml of the drink to the extract, stirred for 30 seconds, observed, repeated until I had added 20ml. Nothing.
I was thinking about it on the way home before I did the test, the ascorbic acid reacts with sodium bicarbonate... so the fizzy reaction between the base and the acid probably forms something else (sodium ascorbate I found later through reading). Probably why it didn't work. I guess I will have to wait a bit longer. Another question answered though :smile:

Update. The 92% layer is starting to turn brown. The layer is kind of iridescent, and I didn't notice the color until I set it on something white. I think that on the next experiment I should measure at what percentages of the original liquid the layers start to form. I think that it would be good to stop now, freeze the liquid and let everything settle, separate the layers and then continue drying them independently. I think that the brown stuff may be a new part of the extract precipitating out.


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OfflineUnderNose
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Re: all you need to know about psilocybin / psilocin extraction. [Re: blahblahblah]
    #9653698 - 01/21/09 07:28 PM (13 years, 1 day ago)

Yeah you have to have lots of shroom to even bother extracting, and the reason you gave there is a good one, condensing down a few months worth of growing into a nice neat little package.
And it would also seem that with all the growing teks like mono tubs that there would be more people trying.

Sometimes I think that if CIA scientists specializing in the synthesis of psychoactive and chemical weapons couldn't do it in 1950s with an secret government run lab then what chance does anyone else have at isolating something pure and stable.
But that's the wrong attitude to have.

The brown precipitate in the 95% could just be fine particulate that you didn't filter out, and its now building up more as the solution is reduced.

The colors you describe about a previous 95% alcohol extraction sound strange(blue ,purple)
The powder stays close to its original colour during and after the extraction, the alcohol starts a light brown and gets darker depending on how much shroom is used and the more it's reduced .....even with heating.
This is without any additives..I.E acids(by lime, citric or ascorbic) or something functioning as a preservative..EDTA
I'm betting its simple as the water in the shrooms caused it. similar to how your 70% extraction that has gone black & blue. Water is just hydrogen and oxygen so it stands to reason that it will cause oxidization.
Well thats just how it seams to me anyway.

But anyway oxidization is only going to reduce potency from a quarter to a half. its not that bad.

Are you trying to evaporating down to powder,?? if you leave it in the alcohol there is almost no oxygen to cause oxidization it, but as a general experiment to see whats what, well why the hell not.

As you have probably noticed in your browsing my mad scientist friend has tried a version of the jungle extraction also, but with little to no results.
But again if you have the shroom to experiment with....why the hell not.

Hopefully FF will turn up as it seems he is quite knowledgeable in these regards.

Will try to get some pics up later.


--------------------
LAGM 2.022

:dna::dna:


Edited by UnderNose (01/21/09 10:17 PM)


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Invisibleblahblahblah
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Re: all you need to know about psilocybin / psilocin extraction. [Re: UnderNose]
    #9657258 - 01/22/09 08:51 AM (13 years, 22 hours ago)

(this post isn't meant to sound negative)
I don't think that because the government couldn't do it, we can't. There have been many advances since the 1950's in chemistry. And really the difference between advancing and not is working out new ideas. I'm experimenting for my own entertainment, and for the good of the community. There haven't been many well documented extractions, just methods, and when read all of them it got confusing.

I'm trying to take this one step at a time, and if I can answer the questions I had and work out mistakes I'm satisfied.

Regarding my previous extractions that failed... the extraction from fresh mushrooms was a dark blue color that turned a light purple upon heating. It happened to the 70% that failed as well, it was yellow/brown and turned a light purple. If it were from the liquid condensing, I'd assume that I'd see it in the current 70% extraction. The liquid is about 3/4 evaporated and it's still a dark blue, almost black color. It hasn't cleared or turned purple the way that the failed extractions did. From this observation, I assume that oxidized psilocin turns light purple upon heating.

As for the fine particulate... it is possible that it is gunk. The gunk in the 70% dish turned blue and then black, the same way that a bruised mushroom does. That is why I assume it is the active chemicals. It's still possible that it's bio gunk, the indigo chemical that's produced from oxidation stains cloth when used to filter the mushrooms from the liquid. The same indigo chemical in the liquid could dye the gunk blue/black as it oxidized. I am just making assumptions from my observations. I think I may test a bit today to see.

More updates later.


Edited by blahblahblah (01/23/09 08:48 AM)


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Invisibleblahblahblah
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Re: all you need to know about psilocybin / psilocin extraction. [Re: blahblahblah]
    #9659267 - 01/22/09 04:19 PM (13 years, 14 hours ago)

Wow. I tested 15ml, which is about 10% of the remaining liquid to be evaporated from the 93% dish. I wasn't expecting what happened. It doesn't seem to have lost any potency from dried mushrooms.

Edit: I was suppose to test the 70%, but because of the taste I opted to drink 10% of the dish that had less liquid :smile: (150ml vs 400ml)


Edited by blahblahblah (01/22/09 04:27 PM)


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OfflineTreeMoss
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Re: all you need to know about psilocybin / psilocin extraction. [Re: blahblahblah]
    #9659285 - 01/22/09 04:23 PM (13 years, 14 hours ago)

any pics of crystals.......I was surprised how nice they looked in a simple ethanol extraction with no A/B.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.


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Invisibleblahblahblah
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Re: all you need to know about psilocybin / psilocin extraction. [Re: TreeMoss]
    #9659337 - 01/22/09 04:31 PM (13 years, 14 hours ago)

No crystals yet. I might filter again to see if the stuff floating around is active. I'm staring to doubt my judgment on what it is.


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OfflineTreeMoss
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Re: all you need to know about psilocybin / psilocin extraction. [Re: blahblahblah]
    #9659357 - 01/22/09 04:34 PM (13 years, 14 hours ago)

So what is it that you have....from what I saw they used warm ethanol with fungus, strained/filtered the fungus then lest the crystals form in the bottom then filtered those off.

I would warm it up again and let the crystals form and drop to the bottom without messing with it.

How much fungus did you use?


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.


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Invisibleblahblahblah
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Re: all you need to know about psilocybin / psilocin extraction. [Re: TreeMoss]
    #9659887 - 01/22/09 06:07 PM (13 years, 12 hours ago)

The stuff floating in the liquid isn't crystals. I just filtered it off, reminds me of something from a kitchen grease trap. Very dark and greasy/slimey. I hope this isn't active...
I'll add pics of the filtering later in the original post.


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OfflineTreeMoss
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Re: all you need to know about psilocybin / psilocin extraction. [Re: blahblahblah]
    #9659908 - 01/22/09 06:13 PM (13 years, 12 hours ago)

Ya I'm saying that  in teks that I've seen on the web white crystals form on the bottom......with brown colored booze on top.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.


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OfflineUnderNose
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Re: all you need to know about psilocybin / psilocin extraction. [Re: blahblahblah]
    #9660920 - 01/22/09 08:44 PM (13 years, 10 hours ago)

The stuff does fall to the bottom eventually.
Its just that while evaporating it condenses at the top because thats where the alcohol is evaporating from, if you leave it for a few hours and the concentration of stuff in the alcohol is high it will slowly form on the surface as the alcohol can no longer hold on to it.
It looks so white because its built up on the surface of the alcohol.
If the stuff is poked or the jar moved to quickly it partially redissolves and mostly falls to the bottom.




So you feel your potency loss is minimal, thats good to hear.
How many grams does the math tell you should be in that 15ml of alcohol, and does it feel the same as that many grams?

Quote:

blahblahblah said:
The stuff floating in the liquid isn't crystals. reminds me of something from a kitchen grease trap




My friend Dr Jekyll had the same kind of feeling to and after taking those macro pics he wasn't so sure. Sorry for the procrastinating on uploading pics..
Trying to bring all experiments to a conclusion first.

But heres a little sample, one of the pics that made think that it could be crystalline.

Top down shot of about 300ml in a jar with ??:shrug:?? floating on top


And one good macro close up.  There was more definition in the structure before I moved the jar, alcohol got on it and fucked it up a little.
Some parts look kind of crystalline but Mr Jekyll is also beginning to think that its just grease or fat, it has the look fat in water. Maybe it could be a good idea to remove and test it to see if Dr Jekyll becomes Mr Hyde.


Oh and I also didn't mean my comment about not being able to achieve a stable pure product as a negative one, just that this particular substance Psilocybin is very difficult to isolate because of it being a zwitterion alkaloid. And the related difficulties involved in extracting into a crystal or powder.
I am all for pushing the boundaries, I just wish I had a more solid understanding of Organic Chemistry, and access to more various solvents and chems to be able to do more experiments. Oh well.

Should have more pics and details in a few days.


Edited by UnderNose (01/23/09 06:44 AM)


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OfflineTreeMoss
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Re: all you need to know about psilocybin / psilocin extraction. [Re: UnderNose]
    #9663787 - 01/23/09 09:38 AM (12 years, 11 months ago)

What kind of alcohol did you use?

I wouldn't use less than ever clear.......even then I'd probably dry it.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.


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InvisibleTomandjerry58
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Re: all you need to know about psilocybin / psilocin extraction. [Re: TreeMoss]
    #9664223 - 01/23/09 11:43 AM (12 years, 11 months ago)

I don't know if this will help, but i found this thread at mycotopia... i was going to give it a whirl the next time i tried.

It talks about leaving the shroomage in the solution for around 3 weeks

http://forums.mycotopia.net/feasts-food-drink-tea-mushroom-dosing-magic-extracts/13128-shroom-extraction-teks.html


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Invisiblefastfred
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Re: all you need to know about psilocybin / psilocin extraction. [Re: Tomandjerry58]
    #9664469 - 01/23/09 12:28 PM (12 years, 11 months ago)

Complete extraction with methanol is reported around 24 hours, less with heating.  Ethanol and acetic acid extractions are complete much faster.

I would never leave anything extracting for more than 48 hours tops.  3 weeks is simply foolish.


-FF


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Invisibleblahblahblah
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Re: all you need to know about psilocybin / psilocin extraction. [Re: UnderNose]
    #9664752 - 01/23/09 01:32 PM (12 years, 11 months ago)

No offense taken, I just re-read my post and it seemed like I was getting defensive so I wrote that at the top. The post was for everyone to understand my motives for doing the extraction, and that I'm not concerned with wasting mushrooms as long as progress is made.

Good to see you popped in fastfred.


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OfflineTreeMoss
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Re: all you need to know about psilocybin / psilocin extraction. [Re: fastfred]
    #9664809 - 01/23/09 01:42 PM (12 years, 11 months ago)

Quote:

fastfred said:
Complete extraction with methanol is reported around 24 hours, less with heating.  Ethanol and acetic acid extractions are complete much faster.

I would never leave anything extracting for more than 48 hours tops.  3 weeks is simply foolish.


-FF




Not when it is a tincture, three weeks is about average.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.


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Invisiblefastfred
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Re: all you need to know about psilocybin / psilocin extraction. [Re: TreeMoss]
    #9665214 - 01/23/09 03:09 PM (12 years, 11 months ago)

> Not when it is a tincture, three weeks is about average.

We're not talking about crude tinctures from plant material.

Properly ground with the proper solvents extraction will be complete in 12 hours.


Quote:

Extraction and analysis of indole derivatives from fungal biomass
Jochen Gartz
Vol 34, 1994; 17-22
Journal of Basic Microbiology

[...]
In the cases with aqueous alcohols as solvent a different extraction time for psilocybin (10 min) and psilocin (160 min) was performed (Kysilka and Wurst 1990).
[...]
In this investigation the extraction of psilocin, psilocybin and baeocystin with pure methanol was not completed after 30 min in all species and even 6 hours in analysis of P. cubensis and G. purpuratus. But the full extraction of the alkaloids from all mushrooms was reached after 12 hours. After this time no traces of indole derivatives could be detected after subsequent extraction of the fungal material with aqueous solutions of ethanol/methanol or acetic acid as well as with chloroform for psilocin.
[...]
It is well known that an extraction procedure with methanol needs much time (up to 12 hours) at room temperature (Beug and Bigwood 1982, Gartz 1987, Semerdzieva et al. 1986) or one hour at 45 C (SCOTTOLANO and Lurie 1983) for complete extraction.

[...]
Additionally, the high activity of enzymes of the phosphatase type in the aqueous solutions of alcohols was already described in aqueous mycelial extracts of P. cubensis and other psilocybin containing mushrooms many years ago (BOCKS 1968, Gartz 1993, Weber and Horita 1963). These enzymes were also extracted with the water containing solvents and caused a partial dephosphorylation of psilocybin to psilocin (Tables 1 and 3). By using these aqueous solutions it was also observed that in some cases bluish mixtures have been resulted after extraction as a sign of partial oxidation of psilocin (BOCKS 1968, Gartz 1989a, Weber and Horita 1963).
Casale (1985) described the rapid formation of psilocin after complete dephosphorylation of psilocybin by heating the dilute acetic acid extract. It is now quite clear that the decomposition under these conditions is an enzymatic reaction and was not ca used by the acid alone.





Hopefully this post will lay this long time issue to rest.  I threw a couple other snips from the paper in there just for fun also.

So it is clear that extraction of fungal material with acetic acid or aqueous methanol/ethanol takes 10 minutes for psilocybin and 160 min for psilocin.  Extraction with methanol takes up to 12 hours.

Based on this data (the best available) I suggest that the standard extraction advice should be 3 hours (180 min) at room temp for aqueous solvents and 12 hours for methanol extractions.

This should be more than adequate for finely powdered fungal material, at room temp, with stirring.  Hopefully this will lay the issue to rest.

Questions?  Comments?


-FF


Edit: Here is the link to the paper quoted...
http://www.erowid.org/plants/mushrooms/mushrooms_journal1.shtml


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Invisibleblahblahblah
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Re: all you need to know about psilocybin / psilocin extraction. [Re: TreeMoss]
    #9665255 - 01/23/09 03:17 PM (12 years, 11 months ago)

Original post deleted.

Updated pics in my original post. The extracts are both sitting in my dessication chamber. 


Edited by blahblahblah (01/23/09 04:18 PM)


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Invisiblefastfred
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Re: all you need to know about psilocybin / psilocin extraction. [Re: blahblahblah]
    #9665635 - 01/23/09 04:21 PM (12 years, 11 months ago)

Your link is to the same paper on a different site.  I've reviewed the paper and their data and I'm quite convinced that their time frames are correct.  It's quite clear that they pursued methanol extractions to the full extent for completeness.  If their aqueous extractions weren't long enough it would have showed up in the data.

3 hours should be plenty for the extractions most talked about here.


-FF


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Invisibleblahblahblah
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Re: all you need to know about psilocybin / psilocin extraction. [Re: fastfred]
    #9666161 - 01/23/09 06:00 PM (12 years, 11 months ago)

I saw that.


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