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OfflineMyco-pathic
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Registered: 08/17/21
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Soxhlet Extraction (Solvents and Heat)
    #27432658 - 08/18/21 03:15 AM (2 years, 8 months ago)

I've been diving deep into the Soxhlet extraction to pull out the alkaloids from mushrooms.

Ethanol was my go to solvent at first because its highly polar and with the soxhlet on repeat should be effective as water at extraction, only letting me distil the alcohol out very easily with a lower boiling point (78.3c).

I would like to make this more efficient and possibly reduce the chance of destroying the alkaloids by using Methylene Chloride (39.8c) for its very low boiling point and its some what neutral charge, if I understand the polarities in solvents correctly it should pull out more of the alkaloids from both sides with multiple runs in the Soxhlet. 

  Polar Index + Boiling temps
Water:              10.2 / 100c
Ethanol:              5.2 / 78.3c
Methylene Chloride:  3.1 / 39.8c

See where I am going here? Or am I going mad?  I feel like methylene chloride will pull the most alkaloids from both ranges although needing more extraction cycles but also sitting at a MUCH lower temperature for a long period of time. Ether has even lower boiling point but much worse polar index.

My reason behind this would be to be left with the purest oil in its lightest form so it may be combined with maltodextrin in order to become a powder much more concentrated than simply grinding dry mushrooms to powder. Which then could be made into more favorable edibles and tinctures with a much smaller overall size. 

Edited by Myco-pathic (08/18/21 03:40 AM)

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Offlinegone-pear-shaped
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Re: Soxhlet Extraction (Solvents and Heat) [Re: Myco-pathic]
    #27432754 - 08/18/21 07:20 AM (2 years, 8 months ago)

Psilocybin is a powder that's insoluble in oils.
https://en.wikipedia.org/wiki/Psilocybin#Chemistry_and_biosynthesis

It's soluble in alcohol, but people have better results dissolving it in water. Why not try that?

Also, I think the more modern way of estimating solubility is to check whether the Hansen solubility parameters of the two substances are sufficiently close to each other (3 numbers--a point, within the minimum solubility sphere of the substance). Unfortunately I couldn't find the HSP of psilocybin. Maybe it hasn't been computed yet. That would be a useful and publishable research project, but you'd need pure psilocybin to accomplish it.

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OfflineLeon ForestFacebookDiscord
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Re: Soxhlet Extraction (Solvents and Heat) [Re: gone-pear-shaped]
    #27433999 - 08/19/21 05:46 AM (2 years, 8 months ago)

It would help if you specify what alkaloids you are trying to extract. If I were to assume psilocin and psilocybin just use distilled water. One important factor people should keep in mind is psilocybin is soluble in water while being slightly soluble in ethanol whereas psilocin is soluble in ethanol and slightly soluble in water. You can use either solvent, the solubility is just going to determine how much will dissolve per measure of solvent. As for degrading compound during the process from heat, that isn't gonna happen regardless of what u pick. It would be pretty insignificant.

Edited by Leon Forest (08/19/21 05:49 AM)

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OfflineMyco-pathic
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Re: Soxhlet Extraction (Solvents and Heat) [Re: Leon Forest]
    #27434422 - 08/19/21 11:50 AM (2 years, 8 months ago)

Thanks for this excellent reply!

I was mildly under the impression that Psilocybin what is broken down by our body into the other, I did a little bit more poking around and found out it’s a little more complicated than that I guess I will be mainly trying to extract Psilocybin because it’s much more stable and is the majority of the fruit body. Possibly will do a dual extraction once with ethanol and then finish with water.

Or do you think with the soxhelt and the repeating cycles with ethanol would be sufficient for psilocybin extraction without using water?

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Offlinesimonjester44
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Re: Soxhlet Extraction (Solvents and Heat) [Re: Myco-pathic]
    #27434871 - 08/19/21 05:00 PM (2 years, 8 months ago)

Soxhlet seems unnecessarily complicated, but Leon Forest is right about solvents.  This is why the double extraction is used.  Use both ethanol and water then combine.


--------------------
"Never underestimate the power of friction as a construction adhesive."

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OfflineLeon ForestFacebookDiscord
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Re: Soxhlet Extraction (Solvents and Heat) [Re: simonjester44]
    #27435465 - 08/20/21 01:48 AM (2 years, 8 months ago)

Just boiling, filtering and reducing is sufficient. no need for a soxhlet, its soluble enough to get enough in 1 or 2 pulls.

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OfflineMyco-pathic
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Re: Soxhlet Extraction (Solvents and Heat) [Re: simonjester44]
    #27435780 - 08/20/21 10:08 AM (2 years, 8 months ago)

Soxhelt it’s not complicated at all, it’s used allot in organic extractions. Smells, flavors, concentrates off all kinds.

It’s very automated and guarantees highly soluble solvents are always in contact with the materials. It’s mesmerizing to watch. That’s the only downside, it being automated you will probably still spend your time watching it. 😅

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OfflineLeon ForestFacebookDiscord
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Re: Soxhlet Extraction (Solvents and Heat) [Re: Myco-pathic]
    #27435889 - 08/20/21 11:49 AM (2 years, 8 months ago)

Its usually used in an application where you need to make many passes, like over a whole day. I would use it for something like capsaicin or piperine. it doesn't take that long to pull alkaloids from mushrooms, also the amount you could fit in one soxhlet is miniscule to what u could just put in a 5 gallon pot and boil for 5 minutes.

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OfflineMyco-pathic
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Registered: 08/17/21
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Re: Soxhlet Extraction (Solvents and Heat) [Re: Leon Forest]
    #27435913 - 08/20/21 12:12 PM (2 years, 8 months ago)

Hehehe mine is stainless 1500 ml 😁
4 inch diameter.

It’s a stove top pot.

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OfflineMyco-pathic
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Registered: 08/17/21
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Re: Soxhlet Extraction (Solvents and Heat) [Re: Myco-pathic]
    #27435930 - 08/20/21 12:21 PM (2 years, 8 months ago)

Far left.

Should be here in next 3 days.


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OfflineMyco-pathic
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Registered: 08/17/21
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Re: Soxhlet Extraction (Solvents and Heat) [Re: Myco-pathic]
    #27435936 - 08/20/21 12:24 PM (2 years, 8 months ago)


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Offlinegone-pear-shaped
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Re: Soxhlet Extraction (Solvents and Heat) [Re: Myco-pathic]
    #27435945 - 08/20/21 12:32 PM (2 years, 8 months ago)

Neat! It's clear you mostly want to play with your new toy. There's nothing at all wrong with that. Would you update the thread later to let us know how it goes? You might also want to try an ethanol/water mix.

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OfflineMyco-pathic
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Registered: 08/17/21
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Re: Soxhlet Extraction (Solvents and Heat) [Re: gone-pear-shaped]
    #27435965 - 08/20/21 12:52 PM (2 years, 8 months ago)

Yes so this is overkill I’m not even gonna lie.

However it does add some quality of life.

I grow a lot of shiitake so I dried about 10 pounds growned it up into a fine powder and did some test runs.

We also have a stainless steel Büchner funnel. The main issue we had was all the fine powder creating a seal and it became impossible to filter.

As well as the amount of time you have to boil it in water as water becomes insoluble at some point.

The benefits to this would be pure soluble solvent will always be what is dissolving the material.
As well as the distillation steel we are using allows for multiple attachments you can build whatever you want.
So very similar to bubble bags used for making hash we will be attaching different levels of filtration below The soxhelt. To create more surface area in a vertical arrangement.
Not to mention the Soxhelt seems to do a good job of not letting too much debris through in the first place.

Therefore after all the pre-filtration taking place the final filtration should be much more simple.
Also we can keep adding and removing material from soxhelt while the 5 gallon reservoir can create a large size batch.

Idk just my thoughts. Will definitely keep this thread updated as I move forward.

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