Mescaline: Basifying and d-limonene after hot water extraction

[shroombee]

Hi All. I know this post belongs in the Cacti preparation subforum, but I can't post there yet.

I've done plenty of d-limonene mescaline extractions with Peruvian Torch. I only get around 0.6% yield which I believe is low considering the potency when I prepare the Torch as a tea. So perhaps the tek just isn't that efficient or my execution of the tek is subpar. I was thinking of trying a hot water extraction like this:

Pure mesc compared to tea/resin - Preparation - Welcome to the DMT-Nexus

Then continuing with the lime/d-limonene tek. I've read a lot of posts on mescaline extraction and wasn't able to find whether this process has been tried. Apologies if I missed the discussion. Any thoughts before I go ahead?

 

[downwardsfromzero]

does the salt dissociate and migrate over to the limonene, thus contaminating our end product when we salt the limonene with acid?

Salt is polar and stays in the polar phase - the water. Sodium chloride will do; its overall inertness outweighs the minor issue of its somewhat limited (but nonetheless sufficient) solubility compared to certain other salts.

 

[doubledog]

Other than to remove the color, is there any other reason to remove the pH indicator if I don't mind consuming the evaporated product?

To see pure crystals after recrystallization is really nice (at least with sulphuric acid)
But if you don't do re-x, contamination from indicator is minimal, and it's red cabbage, so no problem with consuming it.
Red cabbage is easily accessible for me, so I use it. There are of course other options, nitrazine yellow was used by some nexus members for this purpose.

Pull the water with a syringe, squirt into a second beaker to test the pH. Add the acid drop to the beaker. Pull with a syringe and squirt back into the water layer of the first beaker. Probably overkill!

Yes, it will do it and you do not need liquid indicator. But it's too much work. Sometimes it takes 4 or 5 acid additions to reach desired pH.

 

[Loveall]

2) Warm up the system to increase the affinity of FB mescaline to limonene more than that of water. To know whether this is efficient in practice, we'd like to know:
(a) the affinity of FB mescaline to water as a function of temperature, and
(b) the affinity of FB mescaline to limonene as a function of temperature

To check, I would simply split the tea into two and compare the yield from a first pull for warm vs. cold.

In practice there could be things that hardly partition at all into the limonene unless it is warm, and that stuff can make the yield seem higher than it actually is. But, it is worth a test and would be interesting to know. I warm up the solvent to help the limonene separate so haven't done the room temp pull to compare.

PS: Good job going through what to roughly expect by reducing the water volume

 

[Loveall]

shroombee, here is my list of potential small improvements/modifications/updates to the current published tek (69ron's lime/limo starting with 1:3:0.25 cactus powder:water:lime)

1) Make the initial paste more workable by microwaving in short bursts (make sure it does not overflow the jar when boiling) and stirring to half the initial weight of water (use a food scale to keep track), add 20% of remaining water weight as salt and mix well. This process is will cause some ammonia smell.
2) During the Limonene pulls, warm the jar in a water bath. Mix slowly but well (don't whip it up into a Limonene souffle) and allow resting time for Limonene to sweat out of the paste. You should be able to easily pour off the Limonene.
3) After pulling, let the Limonene rest until it is crystal clear and no new sediment forms (e.g. tiny water drops). Decant off the settled Limonene.
4) Use sulfuric acid drops (e.g. 10% used for aquariums) for water salting and monitor pH shooting for ~6.5. A separatory funnel or color indicator makes this easier. Lower pH could pull lower pKa stuff making the extraction less clean. Since salt is insoluble in Limonene (unlike FB which is soluble in both water and Limonene), one salting is enough, just make sure pH is stable at ~6.5 after further shaking. Skip your arm workout day.
6) Reuse the salted Limonene on a new pull and monitor how many sulfuric drops are needed to salt it to pH 6.5. Keep pulling as long as mescaline FB is coming through (one 25ml 10% sulfuric drop neutralizes about 10mg of FB mescaline, so counting drops at helps know when to stop). The drops should follow a geometric series (ratio of drops between pulls constant, for example 100, 60, 36, 22, 13, 8, 5).
7) Combine saltings and precipitate using dg's water reduction and acetone xtalization. Add acetone slowly and stop when cloudy. Adding excess acetone could precipitate other stuff.
8 ) Optionally clean up further with more re-Xs
9) The biggest shiniest xtals I've seen appear after dissolving in water and letting that slowly evaporate over time.

I'm sure I'm missing stuff. Also, some of this could be wrong. The microwaved paste is stinky (likely ammonia from plant stuff breaking down) and is hot/caustic, I have used mason jars without issues, but each person should make their own decision after understanding the process. To the best of my knowledge it works well for me based on trial and error. Cheers.

 

[shroombee]

doubledog, how many mg of the red cabbage powder would you use in, say 100 ml of salting water? I bought some powder on Amazon and it doesn't come with any instructions. :?

To check, I would simply split the tea into two and compare the yield from a first pull for warm vs. cold.

In practice there could be things that hardly partition at all into the limonene unless it is warm, and that stuff can make the yield seem higher than it actually is. But, it is worth a test and would be interesting to know. I warm up the solvent to help the limonene separate so haven't done the room temp pull to compare.

Easy enough - will do.

PS: Good job going through what to roughly expect by reducing the water volume

Thanks for teaching!

here is my list of potential small improvements/modifications/updates to the current published tek (69ron's lime/limo starting with 1:3:0.25 cactus powder:water:lime)

So do you think it's better to stick with the paste tek, or extract to a tea first? I can run experiments on both if there isn't a generally agreed upon answer. But the reason I started this thread was to gather perspectives on hot water extraction then doing lime/limo. And with some other reading I've done, I'm thinking several cold water extraction pulls over a longer period of time might actually be the most convenient from a labor perspective. I don't mind if it takes two weeks (for example) to do all the pulls. Then reduce the tea and proceed with lime/limo.

 

[doubledog]

I would make a concentrated solution with water and use 1ml or even less for 50 ml of water for salting. You don't need strong colour of the water, just enough to be able to see it.

 

[Loveall]

So do you think it's better to stick with the paste tek, or extract to a tea first? I can run experiments on both if there isn't a generally agreed upon answer. But the reason I started this thread was to gather perspectives on hot water extraction then doing lime/limo. And with some other reading I've done, I'm thinking several cold water extraction pulls over a longer period of time might actually be the most convenient from a labor perspective. I don't mind if it takes two weeks (for example) to do all the pulls. Then reduce the tea and proceed with lime/limo.

Either should work well. At some point it becomes a matter of personal preference. I learn with a feedback loop, reading to understand, testing in practice, and then going back to reading. Things become clearer as time goes on and each failure is an opportunity to learn.

One important thing that doubledog helped me see is how much mescaline solubility is affected by other plant stuff. I'm sure this has an effect on the partition coefficient too. In biology, many plant compounds fit together and like to stay in solution - I guess that makes it easier for biological transport. Salvinorin is a striking example of this, with IPA solubility changing a lot if green plant stuff is present. This plant stuff can be destroyed/degraded/removed by a simple dry, a freeze cycle, heat, acid, base, pre-washes. Each thing can affect solubility, the partition coefficient, and the TEK itself. These are not always big effects, but I think it is good to be aware of them.

A fun mental experiment is thinking of oxygen solubility in blood. With fresh blood it would be high. However, denature hemoglobin protein (e.g. a simple heat cycle) and the solubility would drop dramatically I think.

As you can imagine, there are many layers to plant extraction. It is a complicated system, but we do try to simplify it and make somewhat robust TEKs that work to first order.

 

[shroombee]

Quest for most potent cactus - from seeds with help of pereskiopsis grafting - Cultivation - Welcome to the DMT-Nexus

M-malate is a clear white solid composed of needle-like crystals. It is not hydroscopic. It is very soluble in water, insoluble in ethanol and isopropyl alcohol.

Given that mescaline malate is insoluble in alcohol, would it help to clean the cactus with cold dry IPA before proceeding with either water extraction or paste tek? Sort of a defat, but not with a polar solvent.

Perhaps do a few 24 hour pulls in a sealed container in the frig or freezer to remove some of the non-mescaline compounds. We know that the 99% IPA resin/tar tek is mostly ineffective for pulling mescaline, but it does pull a lot of dark green/black gunk that evaporates down to tar. Maybe follow up with a few cold dry acetone pulls? drnocturne didn't say whether mescaline malate is soluble in acetone.

I assume by clearing out that gunk first, our subsequent extraction processes might be much more efficient. I'd be curious to see what a water extraction evaporates down to if the gunk was cleared out first. Or perhaps the mescaline malate would precipitate with the addition of acetone to the cleaner tea?

Just stuff I woke up to this morning. :roll:

 

[Loveall]

How the extraction proceeds after washes would be interesting. It could be easier to do and move the mescaline into the solvent later on. Or, it may not be that different and not worth the effort.

Acetone washes should be fine. I tested warm acetone on cactus powers once and no perceptible mescaline came through.

 

[doubledog]

Hot water extraction is very effective and probably the best (except annoying water reduction, I really do not like that).
It's not that clean work, you need to work with some emulsion, when reduced tea is based and mixed with nonpolar. I found out that when you base reduced tea and let it react till soluble mucilage hydrolyse and it becomes less snotty (this take at least one day), only after that you add nonpolar, emulsions are minimal.

Pre-extraction with IPA or acetone is not worth the effort imo.

Mescaline will not precipitate from tea, when acetone is added, this was tried and don't work.

 

[Grey Fox]

Yes, reducing the raw cactus material down to a tea (water based extraction) just makes so much sense because of how simple and foolproof it is. The beauty of that process is in how simple it is to concentrate large amounts of cactus material down to a few ounces of liquid to consume. It is a wonderfully reliable and effective method. It works everytime, as long as the cactus is good. Full spectrum and all.