Psilocybin Extraction Problems

[DidMyTest]

SWIM tried to extract the Psilocybin of 4gr dried Shrooms. SWIM covered the "powdered" (SWIM dried them with silicate dry gel, but SWIM can't get them to 100% powder) Shrooms with 90% Ethanol and let them rest for a few days near my heating. SWIM filtrated the first load and did the same process two more times. After that SWIM reduced the whole solution to the half amount and stored it in the fridge. After two days there was a white layer on the bottom and some crystal like shapes on top of that layer. SWIM transferrred the remaining solution into another flask and dissolved the layers with fresh ethanol. after evaporating the new mixture and combining the residues SWIM got some brown sticky material like glue. This material SWIM dried on the heating for 2 days and the output was some brown hard stuff with a consistency like melted shugar. SWIM tried to smoke this with a pipe but SWIM got no effects at all.

So a few questions:
1) Is it necessary to wash it with s.th. like naptha to get rid of impurities
2) Why is it brown and doesn't look like needles of a crystal
3) Is the bottom layer just fat/impurities and just the small things above it the crystalls
4) SWIM found a instruction where the powdered shrooms firstly get washed with acetone. But Acetone is polar like ethanol so SWIM doesn't get why the Active Substance doesn't dissolve in Acetone (Albert Hoffman tells this). Also SWIM doesn't know if its better to use Acetone or Naphta (like Albert Hoffmann did)
5) Does anybody know someone who has really smoked the crystalls and notices effects

PS:
Swim used the first Tek:

deoxy.org | E=±mc²=Thé Ðëòxÿríßøñµçlëìç HÿÞêrdïmèñsîøñ

deoxy.org

PS2: Swim noticed s.th. like snowflakes swimming in the rest of the solution which is still in the fridge (so maybe he should reduce it more and place it longer in the fridge)

 

[benzyme]

if you want an answer, quit SWIMming. we all know you did it.

 

[dg]

first off, its hard to get appreciable amounts of extract from such a small starting amount

second, the actives are fairly soluble in polar solvents, so a Long simmer may contribute to more colored impurities being pulled out.

years ago i achieved white crystals after extracting from 2-4oz
ground material, stired on low heat for 30 minutes, vac filtered thru DE, and washed the pulp again w/ stiring for 30 minutes
reduced the polar solution until crystals crashed out, filtered and dried

the extract was active, but at i higher dose than i expected, leading me to believe a large portion of the white glassy crystal was something other than psily

edit out all the swim stuff, and Benz might be of help

welcome aboard btw

 

[benzyme]

something to think about: we use ethanol in biochemistry to precipitate proteins.
fungal carbohydrates (or any carbohydrate, for that matter) are also very soluble in alcohols.

shulgin was undoubtedly wrong (I know, hard to believe), the "crystals" from a soxhlet extraction are not pure psilocybin by any means.

 

[Infundibulum]

The tek in deoxy is bunk - actually no, it is downright a misleading and mischievous tek designed to bring despair to those who fail to reproduce its claims. You're really not going to get crystals like the ones pictured and most certainly you're not going to feel an effect by smoking them. Ethanol extracts extract all sort of stuff from the mushroom mass. While ethanol evaporates and the extract condenses, white crystal-like stuff precipitates, but this is not necessarily actives. I am inclined to believe that these are carbohydrates and/or other sugars from the mushroom mass.

re to your questions:

1) Is it necessary to wash it with s.th. like naptha to get rid of impurities
2) Why is it brown and doesn't look like needles of a crystal
3) Is the bottom layer just fat/impurities and just the small things above it the crystalls
4) SWIM found a instruction where the powdered shrooms firstly get washed with acetone. But Acetone is polar like ethanol so SWIM doesn't get why the Active Substance doesn't dissolve in Acetone (Albert Hoffman tells this). Also SWIM doesn't know if its better to use Acetone or Naphta (like Albert Hoffmann did)
5) Does anybody know someone who has really smoked the crystalls and notices effects

1. no, it is not necesary but it won't hurt. washing the extract with acetone (the actives are insoluble in acetone) will take away the brown colour, leaving white crystalline material. but even if you leave the later to dry, it'll again turn into honey-brown goo. sorry, there're no furter advances to further cleaning this sugary goo without properly extracting and isolating the actives, e.g. A/B, crystallisation and/or chromatography.

2. because that's the way it is. this is what every person that does the tek (even those who clean up with acetone) gets. I suspect that upon evaporation/drying of these white crystals some component in them (sugars?!?!) oxidise to something brown.

3. hell knows.

4. acetone is polar but not as polar as ethanol or methanol. You can try and eat acetone mushroom extract, you won't feel a thing. Even though for polar substances (like mushroom actives) the solubility scale from higher to lower is water>methanol>ethanol>isopropanol>acetone, the polarity of a solvent is not a fool-proof method for determining the solubility of a substance.

5. Nope, this creature does not exist!

Your extract is extremely strong as is and I suggest you try them to see for yourself. The only drawback is that is is hard to measure accurately, but of you mix it with some flour to make it more manageable you'll get around it.

 

[Dozuki]

if you want an answer, quit SWIMming. we all know you did it.

This cracked me up =P

 

[DidMyTest]

Ok, thx a lot guys, a few more questions:

1) Is it a problem to wash the goo with acetone now or does it just work at the beginning of the extraction?
2) Why doesn't anybody extract it with water if it is so soluble in water?
3) Did I get it right, that DMT is vaporizeable because it has a low melting point (44,6–46,8 °C) and psylocybin gets destroyed before it starts to melt (220–228 °C)?
4) How to do the purification with chromatography?

That's how I think it works:
You solve the brownish goo in a solvent. Hang a piece of paper into the solvent (Paper chromatography - Wikipedia) and the solvent moves up the paper. Because of the different physical properties some materials go further than other's. I let the paper dry and cut a thin stripe away. This stripe I divide into sectors and check it with Keller's. After knowing which sections are active I can cut the inactive parts away on the main paper. The active parts I solve again in the solvent for a few hours.I remove the paper and let the solvent evaporate.

5) Do I get it off the paper again?
6) Does the paper soak all the solvent/how much paper do I need for lets say 100ml of ethanol.
7) How exactly is Keller's mixed? I know conc.H2SO4 + FeCl3 + conc.C2H4O2 but not the ammounts and if I can just mix it.

Yeah I know the impurities don't really matter, but I think it's fun to get it pure. And maybe the new skills can also be handy to get super pure DMT.

 

[benzyme]

Ok, thx a lot guys, a few more questions:

1) Is it a problem to wash the goo with acetone now or does it just work at the beginning of the extraction?
2) Why doesn't anybody extract it with water if it is so soluble in water?
3) Did I get it right, that DMT is vaporizeable because it has a low melting point (44,6–46,8 °C) and psylocybin gets destroyed before it starts to melt (220–228 °C)?
4) How to do the purification with chromatography?

That's how I think it works:
You solve the brownish goo in a solvent. Hang a piece of paper into the solvent (Paper chromatography - Wikipedia) and the solvent moves up the paper. Because of the different physical properties some materials go further than other's. I let the paper dry and cut a thin stripe away. This stripe I divide into sectors and check it with Keller's. After knowing which sections are active I can cut the inactive parts away on the main paper. The active parts I solve again in the solvent for a few hours.I remove the paper and let the solvent evaporate.

5) Do I get it off the paper again?
6) Does the paper soak all the solvent/how much paper do I need for lets say 100ml of ethanol.
7) How exactly is Keller's mixed? I know conc.H2SO4 + FeCl3 + conc.C2H4O2 but not the ammounts and if I can just mix it.

Yeah I know the impurities don't really matter, but I think it's fun to get it pure. And maybe the new skills can also be handy to get super pure DMT.

now we're talkin'... he said chromatography.
see? I like this guy already 8)

1) acetone won't do much for this kind of extraction, not in the initial steps anyway
2) people actually do water extractions..it's called tea.
3) psilocybin doesn't break down at its m.p., it decomposes at its theoretical boiling point.
4) what you described is the analytical side of simple chromatography. to do preparative chromatography, you need a column of some sort, and a stationary phase, usually silica or alumina. the principles are similar (you can pretreat your sample with a reagent, usually ehrlich's reagent and/or dragendorff's) and you elute the solvent through wetted silica or alumina, using a binary or tertiary mobile phase (that is, two or three solvents). chloroform, methanol, and ammonia (3:2:1.5) is an effective mixture.
5) and 6) paper chrom is more for analytical work, not so much product recovery.
7) google for pdf: Clarke's Analysis of Drugs and Poisons

 

[DidMyTest]

2) people actually do water extractions..it's called tea.

So why not start with water instead of ethanol, if Psilocybin/Psilocin is perfectly soluble in water, or isn't it?

4) what you described is the analytical side of simple chromatography. to do preparative chromatography, you need a column of some sort, and a stationary phase, usually silica or alumina. the principles are similar (you can pretreat your sample with a reagent, usually ehrlich's reagent and/or dragendorff's) and you elute the solvent through wetted silica or alumina, using a binary or tertiary mobile phase (that is, two or three solvents). chloroform, methanol, and ammonia (3:2:1.5) is an effective mixture.

Hmm maybe I get a setup but I don't want to spend to much money on a fun experiment and I think all the stuff will cost me around 100-200 €. Is it possible to do it with Paper Chromatography. Or is there a big loss of material/significant disadvantages?

7) google for pdf: Clarke's Analysis of Drugs and Poisons

Hmm interesting book. I've a little bit to less time to read it atm . But I will read some chapters about Psilocybin.

 

[DidMyTest]

This page seems quite interesting for testing purposes:

Erowid Psilocybin Mushroom Vault : The Mushroom Entheogen (2)

The Mushroom Entheogen: The Measure of the Mushroom, by C.B. Gold.

www.erowid.org

Now you told me that the instruction isn't that good anyways, do I get it more purified material when I put the reduced ethanol solution into the freezer and collect the parts which fall to the ground and let them dry, or do I get the same output if I just let evaporate everything (without the freezing step)?

 

[woodwight]

One thing about psilocybin/psilocin is that they oxidize or degrade in contact with air. Ethanol extractions work, but total evaporation must be avoided. Try reducing the extract to a few small shots. I usually just make a tea, acidified with citric acid (very important). Adding citric to a blueish tea turns it red. Red coloration of shroom extracts is a good sign. The tea can be reduced to syrup and mixed with honey for very convenient and enjoyable dosing with negligable loss in actives.

Oh, the crystals in an ethanol shroom extract are sugars and metabolic stuff.

Hope this helps

ww

 

[benzyme]

One thing about psilocybin/psilocin is that they oxidize or degrade in contact with air.

not so much psilocybin, it is stable.

I did a methanolic extraction of aborts, filtered the light amber colored solution.
rotavap'd it in a few mins to relative dryness; what remained was a layer of white mass coating the flask. I added hot tea to the flask, then drank it.
'twas very potent.

there's really no need to acidify anything, but it's a matter of preference. the supposed conversion to the parent compound won't occur without some applied heat in acidic solution