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Psilocin extraction help
- Thread starter User_7
- Start date
I'm not sure, maybe just a feeling. Maybe it's because some let on that it's simple, but withhold information. Maybe they really don't know...
A while ago DMT extraction used to be a mindfield (see what I did there). Once upon a time there was no simple pf tek for growing mushrooms, and the original form is very out of date. I guess I just feel that kitchen chem psilocybin extraction is still in it's early days, or that there is less need for it compared to extracting DMT or mescaline, so it gets less attention.
A while ago DMT extraction used to be a mindfield (see what I did there). Once upon a time there was no simple pf tek for growing mushrooms, and the original form is very out of date. I guess I just feel that kitchen chem psilocybin extraction is still in it's early days, or that there is less need for it compared to extracting DMT or mescaline, so it gets less attention.
..i just want to mention that no one here has yet actually posted doing the actual 'Hoffman technique' which is the one i know has worked in this context (i.e. vapourisable...relatively pure for oral purposes is not so hard, but the blue grey crystal is more illusive)..the OP changed around order of procedure, which i think could make a difference.. also as i said somewhere, the repeating of the steps leads to greater purity..each step in the Hoffman method is not necessarily going to be efficient enough from a single wash..
the thing about extraction generally is that it usually takes some 'working', by that i mean that, for instance, once you move away from something like MHRB, which has had 'teks' developed, extracting dmt from different genera of plants doesn't always conform to the same formula exactly, and requires adaptation..psilocybin, being a slightly more complicated molecule, is likely to require more attention in procedure than a standard dmt extraction..
but very few seem to have actually tried the method i refer to, which also worked for Jim De Korne.. the elusiveness here i think stems from simply not many attempts, for whatever reasons..
the thing about extraction generally is that it usually takes some 'working', by that i mean that, for instance, once you move away from something like MHRB, which has had 'teks' developed, extracting dmt from different genera of plants doesn't always conform to the same formula exactly, and requires adaptation..psilocybin, being a slightly more complicated molecule, is likely to require more attention in procedure than a standard dmt extraction..
but very few seem to have actually tried the method i refer to, which also worked for Jim De Korne.. the elusiveness here i think stems from simply not many attempts, for whatever reasons..
Hello friends. First of all, thank you for this and other beautiful mushroom threads full of ideas, experiments, and collaboration by many people such as Orion, endlessness, steppa, Infundibulum , Mindlusion, benzyme, Downwardsfromzero, and many others. I have deep gratitude for all of you.
I think that anti-solvent precipitation of proteins with acetone can help us here. Here is a picture of what I saw this morning (cryatal needles scrape up as loose crystals):
These will need to be analyzed and bioassayed, I don't have that info yet.
This is how these formed (nen888, I'm limited to OTC chemicals).
- Dry and ground mushrooms
- Extract with denatured alcohol from the hardware store (~50/50 ethanol/methanol). I soaked the mushrooms for 12 hours.
- Filter (this was very easy as the pulp likes to stick to itself at this point).
- Add 3x the volume of acetone (I used dry acetone, but not sure if that is required). Strong cloudiness forms. Leave in fridge overnight to settle/incubate. Filter. Pictures of these steps are below. I think we are removing proteins here that make the purification difficult otherwise. Once done, I added more acetone to verify no new clouding indicating protein precipitation was complete.
- Add naphtha. Methanol is not miscible in naphtha and separate layer forms if enough naphta is added. Putting the solution in the freezer increases the methanol rich layer at the bottom, I guess this is just how the acetone-naphta-methanol-ethanol system behaves. The methanol rich layer if strongly fluorescent (green).
- Pick up the methanol layer (I used a syringe) annd dry.
The result is the long needle-like crystals in the picture above. Hopefully, they are an easy and practical way to get we have been looking for. Time will tell.
To scale this up, I think washes with acetone and nabefore extraction could work better. Haven't tried this yet, but the process would look like this (trying to avoid the quaternary system which uses more solvent):
- Ground and dry mushrooms
- Wash powder well with acetone and naphhta
- Extract well (12+ hours) with denatured alcohol and filter
- Add Acetone (+3x the volume). Cloudiness will form as proteins fall out of solution.
- Incubate overnight in the fridge and filter. Add a little more acetone to verify solution stays clear
- Filter
- Dry in shallow pan at room temp
- Collect residue. Ideally residue is long crystal needles.
For reference, below are also pictures of the protein precipitation process starting from the second picture: before adding acetone, shortly after adding acetone, after overnight fridge incubation, after filtering, and the white gunky filtrate left over in the filter).
Will keep this thread updated with any analytical or bioassayed results. Thanks for reading.
I think that anti-solvent precipitation of proteins with acetone can help us here. Here is a picture of what I saw this morning (cryatal needles scrape up as loose crystals):
These will need to be analyzed and bioassayed, I don't have that info yet.
This is how these formed (nen888, I'm limited to OTC chemicals).
- Dry and ground mushrooms
- Extract with denatured alcohol from the hardware store (~50/50 ethanol/methanol). I soaked the mushrooms for 12 hours.
- Filter (this was very easy as the pulp likes to stick to itself at this point).
- Add 3x the volume of acetone (I used dry acetone, but not sure if that is required). Strong cloudiness forms. Leave in fridge overnight to settle/incubate. Filter. Pictures of these steps are below. I think we are removing proteins here that make the purification difficult otherwise. Once done, I added more acetone to verify no new clouding indicating protein precipitation was complete.
- Add naphtha. Methanol is not miscible in naphtha and separate layer forms if enough naphta is added. Putting the solution in the freezer increases the methanol rich layer at the bottom, I guess this is just how the acetone-naphta-methanol-ethanol system behaves. The methanol rich layer if strongly fluorescent (green).
- Pick up the methanol layer (I used a syringe) annd dry.
The result is the long needle-like crystals in the picture above. Hopefully, they are an easy and practical way to get we have been looking for. Time will tell.
To scale this up, I think washes with acetone and nabefore extraction could work better. Haven't tried this yet, but the process would look like this (trying to avoid the quaternary system which uses more solvent):
- Ground and dry mushrooms
- Wash powder well with acetone and naphhta
- Extract well (12+ hours) with denatured alcohol and filter
- Add Acetone (+3x the volume). Cloudiness will form as proteins fall out of solution.
- Incubate overnight in the fridge and filter. Add a little more acetone to verify solution stays clear
- Filter
- Dry in shallow pan at room temp
- Collect residue. Ideally residue is long crystal needles.
For reference, below are also pictures of the protein precipitation process starting from the second picture: before adding acetone, shortly after adding acetone, after overnight fridge incubation, after filtering, and the white gunky filtrate left over in the filter).
Will keep this thread updated with any analytical or bioassayed results. Thanks for reading.
Attachments
beautiful work :thumb_up:
I'm taking the 36 V/-28 VDC switching PS to a repair shop today. A nexian was able to locate an OEM replacement, and its $1500 :surprised
hoping to get this fixed soon, I have alot I want to do, starting with the melatonin-doped samples.
I'm taking the 36 V/-28 VDC switching PS to a repair shop today. A nexian was able to locate an OEM replacement, and its $1500 :surprised
hoping to get this fixed soon, I have alot I want to do, starting with the melatonin-doped samples.
Thanks for the update benzyme. Once you get up and running I'll send you some of these needles too 
Great stuff Loveall, those needles look like something quite different to something you might find after a 'crystals of the gods' tek. The undesirables which have been separated out look like the results of that tek, which we know is bunk, despite what old posts (and now youtube videos...:thumb_dow) say.
The crystals look slightly like NMT or high NMT/ low DMT mixes. I don't know if that should be surprising. I wonder what colours can be produced by intentionally heating or oxidizing the product in solution... But I guess you'd want more to play with before doing any such thing.
The crystals look slightly like NMT or high NMT/ low DMT mixes. I don't know if that should be surprising. I wonder what colours can be produced by intentionally heating or oxidizing the product in solution... But I guess you'd want more to play with before doing any such thing.
..very promising work Loveall:thumb_up:
downwardsfromzero
Boundary condition
Splendid work, the analysis results will be most exciting to hear.
Presumably your method will work with methanol just as well as the denatured ethanol did.
Presumably your method will work with methanol just as well as the denatured ethanol did.
Thanks for the encouragement everone. I'm grateful if I can add a little something to the great ongoing team effort here.
I got 35mg of needels from roughly 2.5g of dry mushroom (it was a a 1/4 split from an original 10g experiment where the other three quarter splits failed). Since the liquid splitting was not very precise numbers could be off, but I would expect around ~1% on repeats.
I just dis this and dried a sample of the up front washes after protein precipitation. While pretty clean, I did not get needles, it is somewhat still gunky. The up-front washes are hard to do (bulky/messy) and don't seem to be that effective. I think it is better to do the cleanup after the alcohol extract.
Also, I'm seeing fluorescence in the acetone. I think this makes sense since any psilocin would go into acetone. Recovering psilocin from the dry acetone residue may be possible (Shulgin used ethyl acetate - sold in the US as MEK substitute - and hexane - Naphta - for a Rx). Also fumaric acid may be able to help purify it (dissolve fumaric acid in the acetone wash, dry, dissolve in water, filter, dry).
DWZ, Yep, methanol should work unless the ethanol is somehow helping get a cleaner extract (e.g. a pure IPA extract is very clean but not active).
Orion, good suggestion about the colors, I'll give it a try when I have more needles. Also want to run TLC vs dry powder.
Here is what I'm trying next:
- Alcohol extract. Split into two batches (A and B).
- A: Naphyha wash (keep bottom layer), acetone protein precipitation, filter, dry, rinse with acetone. Re dissolve residue in denatured alcohol and dry to recover Psilocybin. Work on acetone to try to recover a smaller amount of psilocin (e.g. add naphta, use fumaric acid, etc).
- B: Start with protein precipitation with acetone, filter, add naphtha until bottom layer forms. Freeze to increase volume of bottom layer. Separate out methanol-rich bottom layer and dry (this is a repeat of the previous result where we got needles).
Looking forward to any results on your side KloudQ7.
KloudQ7 said:
I got 35mg of needels from roughly 2.5g of dry mushroom (it was a a 1/4 split from an original 10g experiment where the other three quarter splits failed). Since the liquid splitting was not very precise numbers could be off, but I would expect around ~1% on repeats.
Loveall said:
I just dis this and dried a sample of the up front washes after protein precipitation. While pretty clean, I did not get needles, it is somewhat still gunky. The up-front washes are hard to do (bulky/messy) and don't seem to be that effective. I think it is better to do the cleanup after the alcohol extract.
Also, I'm seeing fluorescence in the acetone. I think this makes sense since any psilocin would go into acetone. Recovering psilocin from the dry acetone residue may be possible (Shulgin used ethyl acetate - sold in the US as MEK substitute - and hexane - Naphta - for a Rx). Also fumaric acid may be able to help purify it (dissolve fumaric acid in the acetone wash, dry, dissolve in water, filter, dry).
DWZ, Yep, methanol should work unless the ethanol is somehow helping get a cleaner extract (e.g. a pure IPA extract is very clean but not active).
Orion, good suggestion about the colors, I'll give it a try when I have more needles. Also want to run TLC vs dry powder.
Here is what I'm trying next:
- Alcohol extract. Split into two batches (A and B).
- A: Naphyha wash (keep bottom layer), acetone protein precipitation, filter, dry, rinse with acetone. Re dissolve residue in denatured alcohol and dry to recover Psilocybin. Work on acetone to try to recover a smaller amount of psilocin (e.g. add naphta, use fumaric acid, etc).
- B: Start with protein precipitation with acetone, filter, add naphtha until bottom layer forms. Freeze to increase volume of bottom layer. Separate out methanol-rich bottom layer and dry (this is a repeat of the previous result where we got needles).
Looking forward to any results on your side KloudQ7.
KloudQ7,
I'm also getting promising results with a slightly different method. I think it would also capture the Psilocin (not just psylocybin) and maybe give higher yields. It also avoids using naphta (some non-polar fats are removed in a different way). First steps are the same as before:
- Dry ground mushroom, extract with with denatured alcohol (12 hours or more), filter.
- Acetone protein precipitation/incubate overnight/filter.
Now instead of adding naphta until a small volume of concentrated fluorescent bottom layer appears, crack out the fumaric acid:
- Dissolve fumaraic acid into the filtered acetone/denatured alcohol solution. 5% of the weight of the dry mushrooms seems to work but may be overkill.
- Dry to get fluffy material that is very easy to scrape up. If it is goopy you can add more fumaric acid, redisolve in denatured alcohol and dry again.
- Dissolve fluffy material in a small amount of water. Excess fumaric acid won't dissolve. Also, remaining clumps of fats will float, you can let this water sit in the fridge overnight to let stuff coagulate and let clumps float to the glass walls where they tend to stick.
- Filter/decant the water to remove the excess fumaric acid and fatty clumps.
- Dry the filtered water (which is fluorescent under UV) to get concentrared crystals. Hope here is that these contain psilo(cy)bin fumarates.
I think I prefer this, because no fluorescence is left behind and no naphtha is used. Not sure how pure the final crystals are or if they are active, would need to biassay and get some analysis going (that's future work). Downside is that if we do get an active salt this way it may not be easy to vaporize. This method may also convert some psilocybin into psiclocin due to the use of acidic water.
I'm also getting promising results with a slightly different method. I think it would also capture the Psilocin (not just psylocybin) and maybe give higher yields. It also avoids using naphta (some non-polar fats are removed in a different way). First steps are the same as before:
- Dry ground mushroom, extract with with denatured alcohol (12 hours or more), filter.
- Acetone protein precipitation/incubate overnight/filter.
Now instead of adding naphta until a small volume of concentrated fluorescent bottom layer appears, crack out the fumaric acid:
- Dissolve fumaraic acid into the filtered acetone/denatured alcohol solution. 5% of the weight of the dry mushrooms seems to work but may be overkill.
- Dry to get fluffy material that is very easy to scrape up. If it is goopy you can add more fumaric acid, redisolve in denatured alcohol and dry again.
- Dissolve fluffy material in a small amount of water. Excess fumaric acid won't dissolve. Also, remaining clumps of fats will float, you can let this water sit in the fridge overnight to let stuff coagulate and let clumps float to the glass walls where they tend to stick.
- Filter/decant the water to remove the excess fumaric acid and fatty clumps.
- Dry the filtered water (which is fluorescent under UV) to get concentrared crystals. Hope here is that these contain psilo(cy)bin fumarates.
I think I prefer this, because no fluorescence is left behind and no naphtha is used. Not sure how pure the final crystals are or if they are active, would need to biassay and get some analysis going (that's future work). Downside is that if we do get an active salt this way it may not be easy to vaporize. This method may also convert some psilocybin into psiclocin due to the use of acidic water.
Update: Fumaric acid helps. So much so that upon trying to do repeats I'm convincing myself that Fumaric acid may have gotten into the first experiment that produced needles without me noting it.
If anyone wants to try this experimental process, this is what works best for me so far:
- Denatured alcohol extract
- Acetone protein precipitation and separation
- Add fumaric acid (5% by dry weight of mushrooms)
- Dry and scrape up white what should be white fluffyness (if gooey more Fumaric acid helps). This fluffy stuff seems like a good result already but has excess fumaric acid and other unwanted stuff.
- Dissolve fluffy stuff in water well. Some fatty stuff and excess fumaric acid won't dissolve, filter that out.
- Wash water with a solvent 2x. I've been using naphta. This seems to defat the product further to give a more crystalline result in the next step.
- Dry the water. Crystal needles should form :d . If dryed under low heat in the oven, some gray/blue coloring appears. Room temp slower drying seems to keep things white (a fan helps).
The needles are easy to scrape up and dissolve in water and make it fluorescencent.
That's it for now
If anyone wants to try this experimental process, this is what works best for me so far:
- Denatured alcohol extract
- Acetone protein precipitation and separation
- Add fumaric acid (5% by dry weight of mushrooms)
- Dry and scrape up white what should be white fluffyness (if gooey more Fumaric acid helps). This fluffy stuff seems like a good result already but has excess fumaric acid and other unwanted stuff.
- Dissolve fluffy stuff in water well. Some fatty stuff and excess fumaric acid won't dissolve, filter that out.
- Wash water with a solvent 2x. I've been using naphta. This seems to defat the product further to give a more crystalline result in the next step.
- Dry the water. Crystal needles should form :d . If dryed under low heat in the oven, some gray/blue coloring appears. Room temp slower drying seems to keep things white (a fan helps).
The needles are easy to scrape up and dissolve in water and make it fluorescencent.
That's it for now
ducdevil
Rising Star
as an observer of this thread, i am fascinated and really interested.
a lot of what i am reading, however, is a bit more vague than the standard "teks" we have posted.
any chance, eventually, this can be posted as a tek which can be more easily followed?
thanks so much for all the diligent work and experimentation! :thumb_up:
a lot of what i am reading, however, is a bit more vague than the standard "teks" we have posted.
any chance, eventually, this can be posted as a tek which can be more easily followed?
thanks so much for all the diligent work and experimentation! :thumb_up:
ducdevil said:
For sure, this is all experimental at this point and the process is not set. Once/if we get a few repeats, yields, bioassay, and analytical results a TEK can be written up.
Of course this whole thing could fall apart (e.g. if the needles are not active). Time will tell, but so far it is looking promising.
KloudQ7 said:
There very well could be. After the protein precipitation I think there may be different paths to get to the final goods. I'm sure there are better ways than what is proposed now. For example if water in the alcohol/acetone is removed/manged well, using Xylene may crash out the fumarates (Xylene may help tie up the methanol molecules since they are miscible).