Feedback Wanted: Extraction of Psilocybin/Psilocin with Acetic Acid

[USA4ME]

A friend of mine ask me to post this for him due to his computer crash. There was a good study (old) done on extraction of Psilocybin/Psilocin and posted at Erowid Mushroom Vault : Journal Article : Extraction and analysis of indole derivatives from fungal biomass, by Jochen Gartz, 1994

It appears Acetic acid is a good/safer second choice in the extraction even though yield will be sightly less but safer and more natural than methanol. He is willing to give up some yield for a more natural/safer extraction process and considering there is not a major lose of Psilocybin and a gain of Psilocin.

QUESTIONS:

1. Is this Tec still a good one or is there a newer/better one?
2. Would you dry the Acetic acid almost completely and then put the left overs in Everclear and store in the freezer w/o O2 present?
3. Would a Soxhlet device be a good choice for extraction?
4. Can a Soxhlet device be used for extracting DMT and also Mescaline using safe materials?
5. Would a used CELL DISRUPTOR be a good choice in making material more exposed to the acid?
6. Is there any other lab equipment needed?

Thanks for any replies

 

[GOD]

Extracting things = powder them and use the right solvent . The hard bit is cleaning extracts .

Methanol leaves a slimy yellow gunge with crystal like lumps .

If you are looking for a clean experience that comes on fast why not just make a tea ? = powdered mushrooms put into 70 C water and then when its cool enough to drink filter it through a coffee filter . A few sips can come on in a few minutes and be as clear as things from a lab .

 

[USA4ME]

Thanks, it looks like the tea method (with alcohol) is the way to go after reading much about extraction, even though the more complex ways appear to give a bit better experience. My friend said he would try the alcohol extract and report back later.

 

[EternalPeace]

This is something I am interested in. I look forward to hearing about your friend's results.

 

[1ce]

A friend of mine ask me to post this for him due to his computer crash. There was a good study (old) done on extraction of Psilocybin/Psilocin and posted at Erowid Mushroom Vault : Journal Article : Extraction and analysis of indole derivatives from fungal biomass, by Jochen Gartz, 1994

It appears Acetic acid is a good/safer second choice in the extraction even though yield will be sightly less but safer and more natural than methanol. He is willing to give up some yield for a more natural/safer extraction process and considering there is not a major lose of Psilocybin and a gain of Psilocin.

QUESTIONS:

1. Is this Tec still a good one or is there a newer/better one?
2. Would you dry the Acetic acid almost completely and then put the left overs in Everclear and store in the freezer w/o O2 present?
3. Would a Soxhlet device be a good choice for extraction?
4. Can a Soxhlet device be used for extracting DMT and also Mescaline using safe materials?
5. Would a used CELL DISRUPTOR be a good choice in making material more exposed to the acid?
6. Is there any other lab equipment needed?

Thanks for any replies

1. I wouldn't use it.
2. One does not simply 'dry' acetic acid, IIRC it azeotropes at a very low purity; making water removal a joke.
3. It's a good choice for (some) extractions, yes.
4. I would not use a soxhlet for DMT. Honestly I'd boil the bark directlty in the flask setup for reflux. No point in using the sox.
5. A CELL DISRUPTOR works well, so does a better solvent. Have you seen prices on these machines? Also search for 'sonic homogenizer' for more resulters.
6. Why not try a different method more practical for your needs?

 

[benzyme]

will attempt another (my fourth) extraction soon.
the methanolic extraction remains the simplest, the product is actually off-white and resinous, a tea made from it gives a quick onset/short duration experience.

 

[1ce]

will attempt another (my fourth) extraction soon.
the methanolic extraction remains the simplest, the product is actually off-white and resinous, a tea made from it gives a quick onset/short duration experience.

Nice probe

What are your thoughts on converting psilocybin to psilocin and pulling with ether?

Seems pretty straight forward.

 

[benzyme]

not straight-forward.
I've mentioned in several threads: across the pH range, psilocin has at least one side group carrying a charge (which is why it cannot exist as a free base), and that allows for electrostatic interactions with other biomolecules.

salting with a dicarboxylic acid may improve stability, but a simple a/b doesn't easily isolate psilocin, and it certainly isn't crystalline as a basified extract.

 

[1ce]

not straight-forward.
I've mentioned in several threads: across the pH range, psilocin has at least one side group carrying a charge (which is why it cannot exist as a free base), and that allows for electrostatic interactions with other biomolecules.

salting with a dicarboxylic acid may improve stability, but a simple a/b doesn't easily isolate psilocin, and it certainly isn't crystalline as a basified extract.

The process I was reading used glacial acetic acid to extract with and convert to psilocin at 70C. Then the psilocin was removed with ether and removed under a vacuum.

 

[benzyme]

I've read the same procedure (Casale 1981) (the extract was also recrystallized with boiling hexane, and purged with inert gas)

acetate complexation will not protect the molecule from autooxidation, which is why acids like tartaric and maleic are used, or alternately, ascorbic.

 

[1ce]

I've read the same procedure (Casale 1981) (the extract was also recrystallized with boiling hexane, and purged with inert gas)

acetate complexation will not protect the molecule from autooxidation, which is why acids like tartaric and maleic are used, or alternately, ascorbic.

I see, so if the proceedure was adjusted to prevent oxidation then there shoukdnt be any issues. I have an inert line.

 

[benzyme]

I'm skeptical that a simple hydrolysis with dilute acid isolates psilocin, but have at it. I'll do the same with a dicarboxylic acid, I also have argon.

when I have enough material to work with (and the motivation), I need to implement (on a preparative scale rather than analytical) strong cation-exchange chromatography. this is a pure charge-based separation technique, definitely not straightforward either; some stationary phases work better than others, and pH changes need to be monitored.

 

[1ce]

Couldn't nitrogen be substituted for argon? Despite an air-gas facility being nearby, ANDZ numerous welding suppliers, argon is relatively expensive in my part of the world.

I can't comment on my thread in the extraction section. I've got a couple homogenizers; But dumping everything into a flask at reflux while I was at work was more than sufficient.=]

^Not to encourage irresponsibility by anymeans. I had someone home to keep an eye on it while I was away.

 

[benzyme]

obviously, argon is denser. it sits concentrated on the surface. nitrogen, well..air is 78% nitrogen.in a vessel, it takes up space, in lower concentration.if nitrogen is cheaper, just use that. argon is the third most abundant component of air, or course it's more expensive..but it's also best for purging a vessel.

 

[1ce]

obviously, argon is denser. it sits concentrated on the surface. nitrogen, well..air is 78% nitrogen.in a vessel, it takes up space, in lower concentration.if nitrogen is cheaper, just use that. argon is the third most abundant component of air, or course it's more expensive..but it's also best for purging a vessel.

Yeah, difference is I have an nitrogen generator. When I don't mind the noise it's extremely disposable. Argon sounds pretty useful for chemical storage thanks to its density. I.E. diethyl ether bottles. I guess nitrogen would leave the potential to not fully remove oxygen unless it was vented in near the bottom.


Welders are a dime a doezen here, perhaps I can get an argon gen or something that'll make it more available to me. Hell even someone with a comercial discount

 

[USA4ME]

will attempt another (my fourth) extraction soon.
the methanolic extraction remains the simplest, the product is actually off-white and resinous, a tea made from it gives a quick onset/short duration experience.

As far as the CELL DISRUPTOR vs. sonic homogenizer goes, from my searches it looks like the CELL DISRUPTOR is considerably cheaper. There is one called Genie they classify as a cell disruptions/homogenizations and claim it is economical as they describe below. One can be bought for under $500 from the right place.
Economical. Performance comparable to expensive ultrasonic cell disruptors/homogenizers. Compares favorably to Mini-Bead Beater*.

Personally if I ever did an extract I would rather use something (disruptor) to get the material as fine as possible, which I assume is the goal (benefit) in most extracts and then use a natural solvent like alcohol-EverClear. I know the alcohol is not the best compared to methanolic extraction. I would think your just helping your alcohol extract a bit better with the disruptor. I had not heard of one before until I read one of your posts.

On a %percent stand point, how much more can you get with the methanolic extraction v. alcohol?

Also I have looked on this site for recommendations on "hand held" (simple) PH meters to no-avail. Any comments on the ones in $100 range?

Thanks

 

[benzyme]

handheld ones? try 'pen pH meters' from Hanna or Extech. you can sometimes find a great deal on e.bay for Beckman or Thermo Orion pH meters. they make standard industrial meters.

%ages? that's a good question, i don't know if anyone has ever tested methanol vs ethanol yields.

looking at the genie, it looks like an agitator that holds small centrifuge tubes. you'd probably put 1.5 mL of sample solution in each tube, with glass/ceramic beads, and agitate the hell out of them.