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Psilocybin acid degredation Options
 
Creachemist
#1 Posted : 8/21/2019 11:39:23 AM

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I was wondering, psilocybin will transorm to psilocin in acidic conditions, but how does this work with an acid base extraction? Because you transform it to salt form but it isn't changing in psilocin (if im correct) i was wondering because i want to perform a psilocybin extraction but was considering a CASA(citric acid saturated aceton) as a purrification method (someting lang a mini acid base)

Thank you for your time and i hope you can help me!
 

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Loveall
#2 Posted : 8/23/2019 4:09:55 AM

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Hello and welcome to the nexus.

Yes psilocybin can convert to psilocin in acidic conditions, especially at higher temps (70C and pH4 for 1 hour is used in the literature) and if certain mushroom enzymes are present (which can depend on the mushroom species).

It's simple hydrolysis I believe,

psilocybin + H2O -> psilocinH+ + H2PO4-

What kind of isolation are you planning to do? If doing an A/B you'll run into several issues. We have shown here you can get something using Xylene after having the water at very high ionic strength (30% ammonium sulphate) and setting the pH near the isoelectronic point for the pull.
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Creachemist
#3 Posted : 8/23/2019 5:21:39 AM

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I was thinking of an acid base because i have experience with such an extraction, however i want my final product to psilocybin because of its stability, so now im thinking about a STB extraction or a crude extraction with later purification, you got any tips for my or a reference for a good tek?

Thank you!
 
Creachemist
#4 Posted : 8/23/2019 5:36:50 AM

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Loveall wrote:
Hello and welcome to the nexus.

Yes psilocybin can convert to psilocin in acidic conditions, especially at higher temps (70C and pH4 for 1 hour is used in the literature) and if certain mushroom enzymes are present (which can depend on the mushroom species).

It's simple hydrolysis I believe,

psilocybin + H2O -> psilocinH+ + H2PO4-

What kind of isolation are you planning to do? If doing an A/B you'll run into several issues. We have shown here you can get something using Xylene after having the water at very high ionic strength (30% ammonium sulphate) and setting the pH near the isoelectronic point for the pull.


After just the tinyst amount of reeding, i think to understand the method

Correct me if im wrong:
You first make a tea of the shrooms, this you clean with a non polar solvent then you adjust de ph to 4 to hit the isoelectric point and then it will behave like freebase en move into the ylene?
Can you also you something else as xylene like naphta or heptane? I dont like the fumes😂
 
Loveall
#5 Posted : 8/23/2019 12:41:43 PM

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In the mass spec, it was psilocin that moved into Xylene in the peak that benzyme found.

While the resulting powder after FASA seems stable, yields are low.

Psilocybin movement onto Xylene was negligable as I remember.

Other solvents you can easily get over the counter used for DMT didn't work, with the possible exception of limonene. That did form clouds, but was never tested.

If you really want to do this without Xylene I would try limonene and first convert everything to psilocin. Using vitamin C may help yield, but not sure. Also work in the dark and quickly.

What I would do after many tests if you really want an "A/B" like process,

- 10g of mushrooms in water, add VitC to pH4 (a few grams), extract at 70C for one our
- Filter and boil for just a few minutes (boiling will help reduce emulsions later from my experience)
- Add 30% ammonium sulphate, a bunch of stuff will crash out, you can filter it
- Adjust pH to about 8.5 (near the pI but not too basic to destroy all the psilocin hopefully - you can try lower pH too maybe like 7, it's about trying to find a mild alkaline place where psilo moves into Limonene but still doesn't degrade significantly while in water)
- Limonene pull
- Fumarate crash/decant
- Fumarate wash in dry acetone

You may get something with this. If you can use Xylene, that has shown to give some psilocin in MS and bioassay, but again yields were low.

Instead of all this, I would reccomend buying cation resin (used for filtering hard water). Then buy tryptophan. Get a cheap two foot tube and make a column. Read the two psilo isolation papers using cation resin from 2010/11. Play around with the tryptophan until you can get it on/off the column. Then copy that process on mushroom extract. Check out the cation resin experiments we are doing in the forum along these lines. I can put the links here if you have trouble finding them.


💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Creachemist
#6 Posted : 8/24/2019 1:00:46 AM

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Loveall wrote:
In the mass spec, it was psilocin that moved into Xylene in the peak that benzyme found.

While the resulting powder after FASA seems stable, yields are low.

Psilocybin movement onto Xylene was negligable as I remember.

Other solvents you can easily get over the counter used for DMT didn't work, with the possible exception of limonene. That did form clouds, but was never tested.

If you really want to do this without Xylene I would try limonene and first convert everything to psilocin. Using vitamin C may help yield, but not sure. Also work in the dark and quickly.

What I would do after many tests if you really want an "A/B" like process,

- 10g of mushrooms in water, add VitC to pH4 (a few grams), extract at 70C for one our
- Filter and boil for just a few minutes (boiling will help reduce emulsions later from my experience)
- Add 30% ammonium sulphate, a bunch of stuff will crash out, you can filter it
- Adjust pH to about 8.5 (near the pI but not too basic to destroy all the psilocin hopefully - you can try lower pH too maybe like 7, it's about trying to find a mild alkaline place where psilo moves into Limonene but still doesn't degrade significantly while in water)
- Limonene pull
- Fumarate crash/decant
- Fumarate wash in dry acetone

You may get something with this. If you can use Xylene, that has shown to give some psilocin in MS and bioassay, but again yields were low.

Instead of all this, I would reccomend buying cation resin (used for filtering hard water). Then buy tryptophan. Get a cheap two foot tube and make a column. Read the two psilo isolation papers using cation resin from 2010/11. Play around with the tryptophan until you can get it on/off the column. Then copy that process on mushroom extract. Check out the cation resin experiments we are doing in the forum along these lines. I can put the links here if you have trouble finding them.




Thank you very mutch after a lot of reading i saw that an A/B is definatly not the way to go but this cation exchange definatly got my attention, because of the fact im not a chemist its pretty hard to place all the date in a logical(to me) order, but im a fast lerener so it should be good

Thank you for your time!
 
downwardsfromzero
#7 Posted : 8/27/2019 7:42:17 PM

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Creachemist wrote:
I was thinking of an acid base because i have experience with such an extraction, however i want my final product to psilocybin because of its stability, so now im thinking about a STB extraction or a crude extraction with later purification, you got any tips for my or a reference for a good tek?

Thank you!
Recovering psilocybin from a sample of biological material is a whole different ball game compared to extracting DMT.

As a home chemist you'll stand literally zero chance of converting psilocin back to psilocybin. This means you'll have to avoid acidic and/or enzymatic degradation to stand any chance of isolating psilocybin. You'd best spend your time getting really good at chromatography and, as Loveall suggests, have a good play around with some ion exchange resins. The twist here would be that psilocybin is a zwitterion so you'd have to look into a somewhat different approach compared to the method as developed for psilocin.

If you really want to achieve your goal then you must have a good dig into the scientific literature to see what the standard procedures for recovering psilocybin for mycological samples actually are. Once you have started doing this we will be more than happy to address any questions that may arise from your reading.




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
 
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