A/B Extraction and Isolation of Psilocybin

Hello All,

I’m curious has anyone in this group has ever tried to extract from the left over substrate with a Sonicator and methanol if so what weee your results and yield.

Thank you in advance

With the half life of psilocin being 30 minutes when in water (referenced above in this thread) and whenever you basifiy the acidic psilocybin solution you create water, would it not be prudent to add some anhydrous MgSO4 to the reaction so as to sequester the water from the reaction as it is generated? It is not soluble in the non-polar that is going to receive the psilocin upon basification.

Be careful with acetone, it is reactive in both acidic and basic environments but is amazing at crashing sugars (and psilocybin). Psilocin is soluble in acetone, psilocybin is not.

Extraction of spent cakes has yielded pretty poor results with a good bit of impurities from the cake itself in my experience. Pretty good way to waste solvents too. Maybe just boil them in acidic water and run with the A/B method. If you think bio psilo yields are not that great, just wait till you see what comes from the cake.

2 Likes

Thanks for the reply zack :facepunch:

1 Like

https://www.reddit.com/r/TheeHive/s/xam8pw1cbX

Someone on reddit claiming to make 4-aco-dmt from cubensis

2 Likes

The process suggested seems reasonable… Ole chatty-bot seems to agree:

To which I went ahead and asked about the other theory of 4-oh-dmt to n,n-dmt:

Thoughts?

4 Likes

Theres definitely better solvent to use other than pyridine. You do need a base to neutralize the acid but the correct base would also help convert any remaining psilocybin to psilocin and start the reaction by breaking the AA apart. Im working on an sop straight from extract thats based off my cannabinoid acetylation sop. I do not plan on making the freebase though.

This explains some of the chemistry behind my sop

1 Like

Definitely keep us updated!

This mushroom extraction dead now? I haven’t seen an updated post in weeks??? I thought this would be the new new :smiling_face_with_tear:

…Extraction is still about 2-3 years away. Laws have been focusing on safe homogenous fruiting bodies. Legally of course, there’s still time.

There’s still time to innovate. Like someone post an acetic acid extraction. I’ve not seen a final product use that, we just know it’s great on hplc chromatograms.

The issue with acetic acid extracts would be the residual taste/smell in a powdered final product. Reducing the acetic may prove useful, however at what cost to yield due to basic reactions?

Methanol is used for the reasons of being relatively cheap, anhydrous or at least very little water present in lab grade solvent, and it’s ability to strip what we want in a time effective manner.

I’m basically done with trying to make money off my setup.

Here is what I learned:

Pressure is an ally. 80psi in Methanol will produce good yields in short time. At room temp.

Pack a column. Fill to the top with Methanol. Clamp lid on. Pressurize to 80psi, with N2, regulated. Check solvent compatibility with gasket type and ball valve seat material. Basically don’t be stupid.

Open ball valve on the bottom after a 20m soak. Drain until liquid slows to dripping not a flow.

Repeat 3x.

Transfer to a pot still, distill Methanol off until a syrup.

Place in vacuum oven and purge until dry.

Blend in bullet blender.

Voila.

No acid, base, or fuckery needed. Just straight Methanol and time and pressure. Simple clean and full spec extract which can be worked with for further refinement with chloroform or other solvents, providing you’re capable and knowledgeable to do so.

7 Likes

If you have a second Methanol reservoir you can even pressurize that to calculate a full 4 columns worth of washes all at once, as long as you can deal with the same volume down line.

Imagine your mushroom biomass as being a stationary phase in chromatography. Now you pass solvent over it and leave the non soluble in place.

You could set up gradients, buffers, so on.

@DiNKLB3RG you done this yet?

Now that I’m just going to be open with it, let’s revive this thread with innovation again.

Think LC column. Biomass is the packing.

Dual piston pumps and solvent gradients to push non polar first, then polar.

Would make cartridge or column tek a real thing.

5 Likes

A picture of a thrown together setup with a solvent reservoir column on the left. I’ve since moved on to a different design, but it did work ok. 22% return on PE mush.

Heat wrap is for methanol recovery from biomass.

I’ve since added a still arm, and PID heat controls. Isolation valves. So on.

11 Likes

@Aurion fantastic writeup and explanation.

Love your work, your attitude, and your ideas.

2 Likes

Imo It doesnt work like that, its more about residence time not extraction solvent volume.
24 hr soak with just enough solvent to cover the biomass is plenty. Even if u did 4x the volume of solvent and soaked the same biomass, it would still take about 24hrs of one soak to get it done.
If u have an ultrasonic bath, u can get that same batch done in 1 hour

4 Likes

Worked well for me, I was looking for throughput and basically evaporated each wash on its own to see that on the 4th wash there was very little coming over.

I’m sure 24 hour soaks, hot washes, soxhlet, centrifuge, or other methods work well, I just found that pressure and multiple washes were faster, with the added bonus of being able to flush a good amount of solvent out of the biomass in the end made more sense for my needs.

Ultrasonic was limiting for me, for the size of unit I have and the subsequent filtration still needed after. I was looking for a high throughput method and this is what I found to be the most time and cost effective for my needs.

2 Likes

Dont get me wrong the way ur doing it is great. I just think that getting a couple bigger vats to do 24 hr soaks, then just use the column to flush and rinse, would speed things up a bit.
Setup the vats over some centrifuges and u could stock up some mushroom tincture real fast.
25lbs per 55gal drum.

I would even opt for a 24hr methanol soak, then perharps a slightly warm ethanol rinse in the columns. That should get it all.

Methanol should be easy enough to seperate from ur alcohol when ur done.

I do come from a bulk production type mind frame, but if you are a oldschool bho blaster then this is a great method. Pretty much same sop, just more forgiving solvent to play with

3 Likes

Working on scaled ultrasonic systems and custom vacuum soxhlets currently. So many ways to skin this

6 Likes

Membranes with pressure are the way to go from my experience and testing

Ultrasonics didnt get me as good of a yield as constantly washing the fruit with fresh solvent while being mixed but to each his own

I have other friends who swear by ultrasonics for extraction but they’re using an isp-3600 or whatever and im definitely not paying a ton of money for a setup like that

1 Like

Jesus tell me abt it. Ultrasonic, centrifuge, membrane. Sets you back like 300k out the gate if going with a built membrane system.

2 Likes

Great feed back fellas I’m glad this thread is still alive… stay posted I’ll provide my feed back shortly…

So this is my process

Step 1:

Grind material into powder

Step 2:

Throw about 20-25 lbs of grounded up material into 100 liter reactor with methanol, turn on the stir with a 3k kw Sonicator and let it run from 2 hrs (letting the sonicator run over night I notice that the rod gets really hot)

Step 3:

Find out the bio via 50 liter Buckner funnel or centrifuge.

Step 4:

Roto out the methanol then into the vaccum oven.

4 Likes