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Washing the Psilocybin Extract Options
 
blue.magic
#1 Posted : 11/16/2018 9:19:36 PM

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I am planning a methanol extraction of P. Cubensis.

The solvent used is very pure and will be completely evaporated using a rotavap.

My concern is that the initial extract might become a sticky mess so the washing might not be effective. Even scraping the sludge off the rotavap flask might be difficult.

Maybe using warm/hot water to dissolve the extract and than washing it in a liquid-liquid fashing might work better?

Unfortunately, there is also little information about psilocybin solubilities. It is insoluble in benzene, chloroform and hexane. It is difficultly soluble in anhydrous ethanol and anh. acetone.

Could DCM be used instead of chloroform?

I think final washing with cold anhydrous acetone and/or cold anhydrous ethanol might be a good idea as these solvents evaporate easily and thus will also dry the extract.

The whole purpose of washing is to obtain somewhat powdery product that can be weighed.

I plan to dry the product in a vacuum desiccator.

Have you any experience with psilocybin extracts and whether they can be turned into a powdery form by washing?
 
 
KloudQ7
#2 Posted : 11/17/2018 1:00:07 AM

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There has been some amazing progress with mushroom extraction by loveall and others in another thread.

https://www.dmt-nexus.me...sts&t=69480&p=11
 
blue.magic
#3 Posted : 11/18/2018 8:19:22 PM

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[quote=KloudQ7]There has been some amazing progress with mushroom extraction by loveall and others in another thread.

https://www.dmt-nexus.me...ts&t=69480&p=11[/quote]

Thanks, I will go through the thread.

I observed Loveall's impressive work, but it is still a work in progress so I just wanted some working approach.

But it seems I will have to experiment on microscale too, before extracting a larger batch.
 
Loveall
#4 Posted : 11/18/2018 8:42:27 PM

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Yep, still very much experimental.

I would recommend you try this in one of your experiments:

1) Add 5x volume of acetone to methanol extract, incubate for a day filter out proteins. Using UV it looks like the actives are still in solution.
2) Add fumaric acid at a rate of 5% of mushroom weight and evap, you should get a fluffy powder at this point Smile. This could already be a powerful product.
3) To clean moar, dissolve in water, filter, wash with naptha (Xylene may wash better). During the first solvent wash you may see a protein pellet form at the water/solvent interface. This is from proteins unfolding at that interface and exposing their hydrophobic/philic sides to each liquid phase and getting trapped at the interphase. Kind of cool. The pro's use this to recover protein pellets in some situations.
4) Add methanol with some fumaric acid to the cleaned up water. Maybe like 1% of the mushroom weight. Dry this. If you use a little heat while drying you may get some blueing (maybe a cool factor for some but you pay with some oxydation).
5) This second fluffy/crystaline stuff may be very concentrated and powerful. Or maybe not, time will tell.

There are probably other/better ways to clean stuff up, but I think the protein precipitation may allow for workable powdery products without the need for column separation. For example this may be interesting based on ongoing work:

A) After step 1. above simply dry. Then wash gunky residue with acetone (which unfortunately removes any psilocin) and naptha. String-like structures remain. Add fumaric acid and water and dissolve everything together. Filter any excess fumaric that does not go into solution. Dry.
B) After step 1 add 10% by volume of tartaric acid. Let sit and see if tartarates precipitate due to common ion effect. This can also be tried before protein precipitation straight on the methanol extraction (but protein salts may crash out first ?).


Cheers and good luck. Looking forward to any results.


β€œ... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
downwardsfromzero
#5 Posted : 11/18/2018 9:31:47 PM

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Quote:
Could DCM be used instead of chloroform?

I can't really answer this except to say sometimes DCM unexpectedly dissolves salts, so be sure to follow the adage of "don't throw anything away until you're sure you know where the goods are" should you decide to use it.


Does anyone here have experience with working under inert atmosphere? It would be my choice for minimising oxidation during the process and it isn't that difficult to rig up if you already have a half-decent lab set-up.
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blue.magic
#6 Posted : 11/19/2018 5:45:03 AM

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Thanks. I've just spent 2 hours reading through most of the current psilocybin extraction threads. Wow that was exhausting...

So many thanks for a summary of your current "state of the art".

Yes I plan using methanol as the primary extraction solvent.

Okay I will synthesize some chloroform for the washing (finally have a use for that 10L canister of strong hypochlorite solution Big grin ).

Apart of being rigorous on drying solvents and fine filtration, I think there won't be any modifications.

I am thinking about making a Keller's reagent to indentify psilocybin (unfortunately, I have not yet found proper ratio of chemicals to prepare it). This has been used by A. Gottlieb (Psilocybin Producer's Guide, 1976). His extraction technique is trivial, using just methanol, then evaporating the solvent to dryness. According to Gottlieb, the purity of this simple extract is 25-50% psilocin/psilocybin (we now know psilocin should be out from the game at this point) - which sounds too good to be true - he however worked with mycelium, not fruits.
 
Loveall
#7 Posted : 12/6/2018 4:08:22 PM

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How's this work going?

I've learned a couple new things while working on this on my side (items 2 and 3):

1) Acetone can crash proteins when added to an extract.
2) Heat can denature and agregate proteins, this can make them easier to crash out. Extreme example is a poached egg. Usually getting above 75F is needed from what I gather, which can be done by 75% ethanol in a water bath.
3) When washing mushroom methanol extract with naphta, a removable protein pellet forms between the inmisible layers (bonus: the methanol may be defatted). I think this is from a mechanism similar to the better known methanol/chlorophorm protein pellet separation.

Hope this helps during your mushrooms extraction adventures. Good luck!
β€œ... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
blue.magic
#8 Posted : 12/6/2018 5:03:21 PM

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Thanks, Loveall, for the tips. I will certainly do the protein precipitation.

I am going very very slowly because having several other projects going. I spent last two weeks just recycling and purifiyng my solvents as well as doing lab cleanup.
 
Loveall
#9 Posted : 12/6/2018 5:12:26 PM

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Trust me I understand. Looking forward to any future news.

I have some promising results I need to reproduce reliably, will send an update when/if I get something that is repeatable.
β€œ... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
Loveall
#10 Posted : 12/7/2018 12:34:41 AM

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Loveall wrote:
How's this work going?

I've learned a couple new things while working on this on my side (items 2 and 3):

1) Acetone can crash proteins when added to an extract.
2) Heat can denature and agregate proteins, this can make them easier to crash out. Extreme example is a poached egg. Usually getting above 75F is needed from what I gather, which can be done by 75% ethanol in a water bath.
3) When washing mushroom methanol extract with naphta, a removable protein pellet forms between the inmisible layers (bonus: the methanol may be defatted). I think this is from a mechanism similar to the better known methanol/chlorophorm protein pellet separation.

Hope this helps during your mushrooms extraction adventures. Good luck!


Here is more info on 1) and 3) and they also have other info on managing proteins (which I think may be important in mushroom extraction). They mention TCA, but I think that can be overcome by using more acteone volume.
β€œ... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
Loveall
#11 Posted : 12/7/2018 4:50:22 AM

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Interesting, TCA is used for tattoo and genital wart removal and available OTC in general. I was not aware of this at first.

However, care should be taken with it, as it can form salts and endup in a hypothetical product. There are protocols out there where acetone is used to wash TCA from the protein
pellet. The thing to do here is to simply stick to acetone for protein precipitation experiments, unless you really know what you are doing.
β€œ... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
Loveall
#12 Posted : 12/9/2018 1:07:39 PM

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PEG can also be used to precipitate proteins. May not be as convenient as acetone and TCA since it can form viscous solutions.
β€œ... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
benzyme
#13 Posted : 12/9/2018 4:47:16 PM

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if anyone sends me samples for analysis, please don’t use PEG. It sticks out like a sore thumb, and takes a while to eliminate from the system.

or clean the sample thoroughly.
thanks Big grin

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