Mescaline sulfate Manske?

[Loveall]

Has anyone tried this before?

- Cacti water extract/filter/reduce
- Add a sulfate salt (e.g. ~20% ammonium sulfate or epsom). Proteins may precipitate.
- Cool down to see if mescaline sulfate precipitates due to low cold water solubility and common ion effect.

Why would this not work? Is it worth a try? Thank you.

 

[downwardsfromzero]

This is a brilliant idea and I absolutely love it! One would have to be aware of the poor solubility of calcium sulfate which would maybe confound initial yield calculations. However, calcium sulfate is even less soluble in hot water so it should be fairly easy to redissolve the mesc sulfate in fresh hot water and filter off the gypsum.

[Sidenote: Does anyone happen to know the solubility of mescaline sulfate in aqueous ethanol of various strengths?]

 

[Loveall]

Thanks DWZ. I'll avoid adding Ca.

I would imagine adding alcohol or acetone would further decrease mescaline sulfate solubility (but other sulfate salts also). We have dg's water/acetone/sulfuric Tek as an example.

Based on this feedback I'll throw some cacti at this and see what happens. I haven't been able to find positive or negative reports on this so far. Cheers.

 

[downwardsfromzero]

Yeah, I saw you'd dug up dg's old tek!

Calcium salts are likely to be present naturally in the cactus.

Even if it doesn't work out, you'll not have destroyed any of the molecule of interest and it would be a matter of the usual procedures to recover it and start again.

So, it would be a matter of dumping magnesium sulfate solution into a cactus tea, both solutions being hot, then, after observing for precipitation, possibly filtering before transferring to refrigeration. Perhaps I'll be able to compare results here soon. Magnesium sulfate has poor solubility in ethanol and is practically insoluble in acetone so bisolvent systems would be largely out of the question, due to precipitation of the MgSO4.

 

[doubledog]

Reducing cactus water too much will lead to very thick solution, full of dissolved cactus mucilage, what most likely will hinder mescaline salt precipitation. Reducing only slightly will not be enough to decrease solubility of m. sulphate.
By adding alcohol to cactus tea, mucilage precipitates.

 

[downwardsfromzero]

Reducing cactus water too much will lead to very thick solution, full of dissolved cactus mucilage, what most likely will hinder mescaline salt precipitation. Reducing only slightly will not be enough to decrease solubility of m. sulphate.
By adding alcohol to cactus tea, mucilage precipitates.

Boiling for long enough breaks down mucilage and also allows some of it to be skimmed off as a foamy scum. This leaves a much less viscous brew to work with, but may depend on the exact cactus species/strain for its level of success.

Adding ethanol will also cause numerous inorganic salts to precipitate, if they are present. This seems likely, as many cactus brews taste pretty damn salty besides the rest of the flavour that most people find so revolting.

If anyone decides to try this idea it may even make sense to add ethanol, filter off the precipitated salts and mucilage, and then distil the ethanol back out of the solution before finally adding the sulfate salt of choice. This would make the the whole process rather less simple, of course, but advantages are relative. If this proved to be a way of avoiding the use of strong-smelling solvents like xylene or even limonene that would be a different kind of advantage.

 

[doubledog]

Reducing cactus water too much will lead to very thick solution, full of dissolved cactus mucilage, what most likely will hinder mescaline salt precipitation. Reducing only slightly will not be enough to decrease solubility of m. sulphate.
By adding alcohol to cactus tea, mucilage precipitates.

Boiling for long enough breaks down mucilage and also allows some of it to be skimmed off as a foamy scum. This leaves a much less viscous brew to work with, but may depend on the exact cactus species/strain for its level of success.

Breakdown products of mucilage are still in the brew and will not precipitate fully even in presence of isopropanol or ethanol in high concentration. After evaporation of alcohol, leftover still holds lot of inactives.

Adding alcohol is very suitable method for producing purified and potent cactus resin, but
I think that concentration of mescaline after these steps would be still too low for successfull separation by introducing sulphate.
But generally, I like this idea and will probably do some experiments in this way.

 

[Infundibulum]

This is a brilliant idea and I absolutely love it! One would have to be aware of the poor solubility of calcium sulfate which would maybe confound initial yield calculations. However, calcium sulfate is even less soluble in hot water so it should be fairly easy to redissolve the mesc sulfate in fresh hot water and filter off the gypsum.

[Sidenote: Does anyone happen to know the solubility of mescaline sulfate in aqueous ethanol of various strengths?]

I concur, great idea!

Whatever can be done to minimise doing those billions of NP solvent pulls from the basified cactus I would consider a victory.

 

[Loveall]

Thanks for the feedback everyone. Will need to watch out for natural calcium sulfates crashing and mucilage preventing the hypothetical precipitation.

I went ahead and did a simple test. Started with 70mg of "mescaline acetate" from the limonene/vinegar tek - the first picture is the result from step 5 in the main procedure after drying the vinegar and scraping. Dissolved that in warm water and filtered it (most of it dissolved well but there were a couple of stubborn tiny specks left). To the filtered solution (second image) and equal amount of ~ saturated ammonium sulfate water was added and cloudiness appeared (promising) and that put in the fridge. The next morning there are clumps in the solution (3rd picture).

I'm not sure what precipitated (it could be anything since the acetone/limo product is only thought to be ~50% pure) so more work is needed. I this just means that we can't discount a Sulfate Manske for Mescaline for now (I'll call it SMANSKE from now on).

 

[Loveall]

For reference, ammonium sulfate is ~40% soluble by weigh in water (~70g dissolves in 100ml of water). The freezing ppint at that concentration is ~0F (-18C) which could remain liquid in a home freezer (depending on the setting).

 

[Loveall]

After filtering and drying the precipitate from the previous post it seems like only brown gunk is present

So, another consideration is that the mescaline sulfate found out there is,

(MescalineH+ and HSO4-)

I think the mescaline sulfate that has low solubility in cold water is really "mescaline bisulfate" (?)

Sulfuric acid pKa is ~2 (for HSO4- and SO4-- equilibrium), so to form mescaline bisulfate and crash it at low temp with common ion effect a low pH (<2) is needed.

As for the theoretical (mescaline)2SO4 salt it doesn't seem to exist in isolation and/or I can't find any reference to it.

This means that a simple water SMANSKE in mildly acidic conditions (pH 3-6) may not work. The gunk obtained could be contaminants from the acetone/limonene Tek (which are a known to be present).

Fortunately I saved everything and can try to lower the pH of the filtrate to see what happens. Using a bisulfate salt to begin with may also make sense.

 

[Loveall]

I tried lowering the pH of the filtrate but the ammonium sulfate is a pretty good buffer. In short, I could not get it to work.

Looking at bisulfate salts they seem pretty harsh
Since salts can end up on the end product this doesn't seem like a good path for future tests.

On the other hand monosodium phosphate is something safer and testable in mild acidic conditions. I may test it one day. Cheers.

 

[downwardsfromzero]

Well, at least you succeeded in crashing out some of the gunk!

It might still be worth trying with MgSO4 as that's less of a buffer(?)


Funny, I bought a bunch of NaH2PO4 a couple of weeks ago. It's very easy to get hold of OTC (for baking); now its purpose may have become clearer...

Noteworthy, perhaps, is that magnesium ammonium phosphate has a very low solubility and is used for precipitating magnesium effectively quantitatively. After ignition to drive off the ammonia the resulting magnesium pyrophosphate can be weighed.

 

[Loveall]

Cool, it would be great if you could test a mescaline PMANSKE one day (P = H2PO4-). I don't have that salt at this time.

Unfortunately, I don't know how soluble it is in cold water, but worth a try in my book.

In other mescaline extraction news, there may be a shortcut for the acetone/water/sulfuric crash that dg discovered.

 

[downwardsfromzero]

Wikipedia lists monosodium phosphate's solubility in water as 59.90 g/100 mL (0°C). That's quite a lot, so I get the feeling it might be quite useful. Especially as it's readily available OTC as a food additive (In Asian/Arabic shops, maybe. Have I said too much?)

Other data:
pH: 4.4 (1 %)
Specific gravity/density: 2360 kg/m³
Hygroscopic
melting point 60 °C (dihydrate)
insoluble in ethanol

 

[Loveall]

Discussed with Mindlusion and 2(MescalineH)SO4 is the salt that forms at mild pH.

In short, this could work with Epson salt, no need to get to lower pH.

Perhaps my original issue was that other stuff crashes too, so the gunk could have a good amount of mescaline. Would need to to a fresh cactus water extract next time. What precipitates after adding Epson salt may well have Mescaline among other stuff.

 

[Loveall]

I started with a "cleaner" extract and things are interesting again.

Starter with the gunk that precipitates after two volumes of acetone are added to a concentrated water cacti extract. After the gunk dried, I redisolved it a small amount of water and let it settle, filtering ant sediment. To this I added epson salt and something white is now precipitating (powdery not long needles though).

 

[Loveall]

I started with a "cleaner" extract and things are interesting again.

Starter with the gunk that precipitates after two volumes of acetone are added to a concentrated water cacti extract. After the gunk dried, I redisolved it a small amount of water and let it settle, filtering ant sediment. To this I added epson salt and something white is now precipitating (powdery not long needles though).

This ended up being gunky powder and a bust, but I have not abandoned this yet.

I think something I overlooked is the starting mescaline concentration that double dog mentioned. It could be very important.

Trying to be a little quantitative let's call:

h: MescalineH+ concentration
c: added SO4--
s: Solubility of 2(MescalineH)SO4. It is related to the equilibrium constant of 2(MescalineH)SO4(s) <---> 2[MescalineH+] + [SO4--] by K = s^3.
r: Recovery ratio of mescaline after precipitation. After precipitation, h - rh of MescalineH+ remain in solution.and c - rh/2 of SO4-- remain.

The equilibrium for 2(MescalineH)SO4 after precipitation is:

(h-rh)^2(c-rh/2) = s^3

Precipitation starts when r>0. The limit case is r=0, which substituted in the equilibrium equation gives immediately,

h^2c > s^3,
h > sqrt(s^3/c)

So, to double dog'ss point, there the concentration of mescaline has to be higher than this value for manske to work.

Let's check what I did in the earlier post above. I dissolved the 70mg of "mescaline acetate" in ~100ml of water. Let's say half was actual mescaline, that gives h ~ 0.001M.

Next, s has been very roughly guestimated at s ~ 0.02M. Finally, the ammonium sulfate I prepared was 2M, so ~ sqrt(s^3/c) = 0.002M.

If this is true, my solution was too dilute for the manske I was thinking of. It needs to start at a higher mescaline concentration, at least ~10x over the minimum I think, and ~20x times than where I started at in the first crude test.

So a point where manske could give good results is ~1g of mescaline (~100g dry cactus) in 100ml of water. There would be a lot of plant material to deal with though since the dry cacti can absorb that water up front. An acetone crash or some other treatment would be needed to get to this concentration of mescaline.

I think I'm going to try again. Perhaps using a concentrated hot water extract add sulfates (mescaline sulfate should stay in the hot solution while proteins and gunk should still crash I believe). Cool and check for new precipitates. Hoping mescaline sulfate crashes while cooling (but other stuff will likely crash too).

Getting a good measurement of mescaline sulfate in cold water could be a helpful to guide here. Does anyone know?

 

[Elrik]

How did I not join this thread in january :lol:
I've used common ion effect to refine mescaline sulfate out of very accessory alkaloid rich cactus hydrochlorides before, the pearlescent flakes I got gave a great trip. I subsequently tried using the same ammonium sulfate concentration to extract it from cactus tea made from a known-good cactus and got nothing, this perplexed me and I tried using mescaline acetate from that same cactus and again got nothing initially, but after months in the fridge some crystals came out. I don't have time right now to summarize my full notes but there is potential and also a warning: the sufficient concentration of ammonium sulfate will also precipitate pectin/protein goo.

 

[Loveall]

How did I not join this thread in january :lol:
I've used common ion effect to refine mescaline sulfate out of very accessory alkaloid rich cactus hydrochlorides before, the pearlescent flakes I got gave a great trip. I subsequently tried using the same ammonium sulfate concentration to extract it from cactus tea made from a known-good cactus and got nothing, this perplexed me and I tried using mescaline acetate from that same cactus and again got nothing initially, but after months in the fridge some crystals came out. I don't have time right now to summarize my full notes but there is potential and also a warning: the sufficient concentration of ammonium sulfate will also precipitate pectin/protein goo.

Thanks Eric, that is interesting. I agree with precipitation of the goo, I can confirm I saw that. I just didn't get mescaline to crash and I think it is because I was too dilute.

The goo (or parts of it) may not be as sensitive to temperature. So, in warm water goo will (hopefully) mostly crash, but mescaline sulfate should not. After filtering and cooling mescaline sulfate will (hopefully) crash under the right sulfate and MescalineH+ concentration.

I think knowing s in cold water would be helpful to setup the concentrations we need. The equilibrium equation in the previous post can re-arranged as,

c = hr/2 + (s^2/h^2) * (s/(1-r)^2)

Guessing s = 0.02M, the attached graph shows how the salt concentration (c) looks as as a function of starting mescaline concentration (h) to crash 90% of sulfates (r = 0.9):

There could be typos/mistakes, and s could be incorrect, but I think it shows qualitatively that the starting mescaline concentration is critical to the process. I think a reasonable place to start would be a concentrated water extract that ways about the same as the starting dry cactus.