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methanol extraction Options
 
Orion
#61 Posted : 6/30/2013 10:28:46 PM

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You're not alone on this crystal mass deal Trickster. I remember seeing a post on a forum where he had a jar full of gunk extracted from shrooms and he left it for a while. Large cubic crystals started to grow on the bottom, they looked very cool, but unfortunately were not active. I believe the thread was on mycotopia but googling it again gets me nowhere.
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dakkapel
#62 Posted : 4/29/2015 1:58:02 PM

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I have some shrooms from which i want to extract the psilocybin. The shrooms are a couple of years old stored in the dark at 10-15C.

When you use methanol. And you evaoprate it in a rotavap. Can you reuse the methanol?
Cause when it reacts with oxygen you get formaldehyd...



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benzyme
#63 Posted : 4/29/2015 3:50:43 PM

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in that scenario, what would be catylazing dehydrogenation? it doesn't occur spontaneously.
and yes, you can reuse the methanol
"Nothing is true, everything is permitted." ~ hassan i sabbah
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dakkapel
#64 Posted : 4/29/2015 7:43:55 PM

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benzyme wrote:
in that scenario, what would be catylazing dehydrogenation? it doesn't occur spontaneously.
and yes, you can reuse the methanol


Seemingly silver and iron and such...
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benzyme
#65 Posted : 4/29/2015 10:30:39 PM

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neither of those are present in a borosilicate vessel
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
1ce
#66 Posted : 4/30/2015 12:42:26 AM

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ftw indeed
 
dakkapel
#67 Posted : 4/30/2015 1:41:21 PM

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After eating 3 gram of dried cubensis there was very little effect.
They are 2 years old. Maybe that is why they are not so strong anymore. They were stored in the dark tough.

So instead of eating 10gram dried... maybe extracting the psylocibin could be nice. But as I go further with studying on this, it seems it is fairly difficult to get a pure result.

Till now the procedure is as follows:

1. grind mushrooms
2. soak in methanol for 24hr
3. doing soxhlet extraction (at 67C? )
4. rotavap
5. Consume


Any comments or ideas are welcome Smile




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benzyme
#68 Posted : 4/30/2015 3:50:21 PM

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when going the extraction route, you really have to fully lyse the cells to get maximum yield/effect. this is very important, because the alkaloids are inside the fungal cells. of course, when you eat them, lysing doesn't matter, because the gut hydrolyzes the fungal cells.

3g isn't much to work with, so thorough lysis is needed.
"Nothing is true, everything is permitted." ~ hassan i sabbah
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dakkapel
#69 Posted : 4/30/2015 4:40:02 PM

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benzyme wrote:
when going the extraction route, you really have to fully lyse the cells to get maximum yield/effect. this is very important, because the alkaloids are inside the fungal cells. of course, when you eat them, lysing doesn't matter, because the gut hydrolyzes the fungal cells.

3g isn't much to work with, so thorough lysis is needed.



There is 30g dried or something.

Maybe couple of time freeze/thaw can help and then grind them?

Problem with the soxhlet will be that also a lot of other particles will be extracted. It will just flow with the methanol through the filters?
Is there maybe a way to do it liquid/liquid?


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1ce
#70 Posted : 4/30/2015 6:38:02 PM

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I suggest builing a dessicator. Dehydrate some epsom salts in the oven. Cut some window screen to fit the approximate size of the dish. When the epsom salt has been dehydrated, dump it into the dish.

Cover with window screen, cut up your shrooms, and place your lid.
 
dakkapel
#71 Posted : 4/30/2015 10:21:01 PM

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1ce wrote:
I suggest builing a dessicator. Dehydrate some epsom salts in the oven. Cut some window screen to fit the approximate size of the dish. When the epsom salt has been dehydrated, dump it into the dish.
Cover with window screen, cut up your shrooms, and place your lid.


And what is the purpose? Conservation of the mushrooms?
I kept the mushroom in a pot with a bag of hydrofile silica stuff they use in cat litter box. We are on the same page in that respect Smile

But to get back to lysing subject. What about cooking with water? Making a tea with it and then use a liquid-liquid extraction. Which solvent could be selective for the psilocibin?


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1ce
#72 Posted : 4/30/2015 11:10:03 PM

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dakkapel wrote:
1ce wrote:
I suggest builing a dessicator. Dehydrate some epsom salts in the oven. Cut some window screen to fit the approximate size of the dish. When the epsom salt has been dehydrated, dump it into the dish.
Cover with window screen, cut up your shrooms, and place your lid.


And what is the purpose? Conservation of the mushrooms?
I kept the mushroom in a pot with a bag of hydrofile silica stuff they use in cat litter box. We are on the same page in that respect Smile

But to get back to lysing subject. What about cooking with water? Making a tea with it and then use a liquid-liquid extraction. Which solvent could be selective for the psilocibin?




I've been experimenting with a methanolic:acid solution with good results. Methanol shows a higher yielding extract, but taking a very long time to complete. Adding a small amount of acid assists in the extraction completing the process in 30 minutes (vs 12-16hrs).

Methanol is preferred as psilocybin is poorly soluble in ethanol. After I filter the shrooms out of the solution I pass it over MgSO4 to remove excess water, centrifuge, and evaporate.

IIRC Benzyme stated water extracts proteins that reduce psilocybin to psilocin (which is readilly oxidized). Evaporation of the methanol has reliably given me an --off-white waxy powder I encapsulate.
 
dakkapel
#73 Posted : 5/1/2015 8:57:49 AM

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[/quote] I've been experimenting with a methanolic:acid solution with good results. Methanol shows a higher yielding extract, but taking a very long time to complete. Adding a small amount of acid assists in the extraction completing the process in 30 minutes (vs 12-16hrs).

Methanol is preferred as psilocybin is poorly soluble in ethanol. After I filter the shrooms out of the solution I pass it over MgSO4 to remove excess water, centrifuge, and evaporate.

IIRC Benzyme stated water extracts proteins that reduce psilocybin to psilocin (which is readilly oxidized). Evaporation of the methanol has reliably given me an --off-white waxy powder I encapsulate.[/quote]

To check if I understand you correctly:
So after lysing the cells. Like freeze/thaw and grinding the shrooms you put them in the soxhlet. Using methanol as extraction solvent together with acid.
Which acid and how many ml acid per ml methanol?

Then after 30min of soxhlet extraction you filter out the pieces of shrooms. Using hydrofile MgSO4 to get out the bits of water.
Then centrifuge... How do you do that?

And you tested the endresult? Smile
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1ce
#74 Posted : 5/1/2015 6:22:43 PM

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I pour the MeOH in the beaker and add the grounded shrooms. (I didn't freeze) and hold the temp at 40C. I add 5% tartaric acid, vac filter, pour over MgSO4, wait 10 minutes, vac filter again, and centrifuge the methanol.

 
dakkapel
#75 Posted : 5/2/2015 4:57:55 PM

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1ce wrote:
I pour the MeOH in the beaker and add the grounded shrooms. (I didn't freeze) and hold the temp at 40C. I add 5% tartaric acid, vac filter, pour over MgSO4, wait 10 minutes, vac filter again, and centrifuge the methanol.



Thank you for the clarification!!
Unfortunately I have no centrifuge. Or do you mean a rotation-evaporator?
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1ce
#76 Posted : 5/2/2015 6:30:38 PM

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Centrifuge, to separate out impurities. It works for DMT, too.

https://www.dmt-nexus.me...aspx?g=posts&t=63466
 
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