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Simple, nearly perfect separation of DMT+NMT with acetone Options
 
moyshekapoyre
#1 Posted : 2/2/2020 10:46:20 AM
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Here's how to separate DMT + NMT + other alks (photo of final separation):

Stumbled upon this experimentally after previously trying with other solvents that didn't work quite as well.

I had some DMT+NMT+? crystals (obtained with an STB extraction of MHRB) which felt to me mostly like NMT (no visuals, but lots of wandering thoughts, vs pure DMT which has powerful visuals and ego dissolution along with a quieted mind).

STEP 1:

I put 5g of the mixed crystals into a 15mL test tube and filled it with room temperature acetone. I had multiple batches of alkaloids so I used multiple test tubes like this. Not all pulls ended up containing the same alkaloids.

Within seconds, multiple layers formed in the test tubes. The tube that I thought contained the more pure-looking-and-feeling xtals gave 4 layers, which included a bottom undissolved white crystal layer (about twice the density of DMT crystals: when you drop them they make a thud sound, and they dry super fast, see LCMS graph), a cloudy little layer above that, then a somewhat dark yellow layer above that, and finally a large light yellow layer.

The other tube which I felt must have more NMT based on how it felt and looked, did indeed form a red layer under the top light yellow layer. This red one is very special and I'll explain that in a bit...

In order to more fully separate and define the layers, I put the tubes in a centrifuge for 5 minutes or so, which also heated them up a bit.

I avoid shaking the test tubes. Once mixed, I can't unmix these layers.

I siphon off the majority of the top layer with a syringe, leaving the bottom layers behind.

I air-dried the resulting 5 fractions separately.

I first vaped the top light yellow DMT fraction--at this point not knowing if it was actually DMT, NMT, or a mix or something else. Surprise: for the first time in almost a year, I've got the effects of pure DMT (not sure if folks have noticed that Mimosa hostilis has started containing more NMT, both in Mexico and Brazil).

I then vaped the red fraction, and indeed, I got pure NMT effects (happy, wandering thoughts, not very psychedelic), although since NMT seems to have a higher receptor binding affinity than DMT, I can't state with certainty how pure the NMT is. This NMT did work to activate the "Metta" love molecule in Acacia confusa, btw. LCMS graph for the red NMT fraction (Benzyme confirms it's NMT).

I then vaped the other 3 fractions I mentioned. Each felt sleepy/dreamy but had different effects. None felt like DMT or NMT. The bottom layer that remained undissolved (LCMS graph again) left me feeling a bit in a dream state for a while after vaping it, tho I could still function. The layer above that, the cloudy one (LCMS graph), transported me to a realm of what seemed like many confused beings all sort of swimming pressed against each other amorphously. They reminded me of maybe people who had died but not moved on--when I sent these beings love, they transformed into my wife(!). The dark yellow layer (LCMS graph) had some type of dreamy visions but I can't recall much about them.






STEP 2 which might be necessary:

After letting the top DMT layer dry one time, I noticed that my separation didn't seem perfect, because I had non-uniform crystal formation as you can see in this photo: https://ibb.co/S6ds3j9

So, the simple extra purification step was just to scoop out the minority formations and set those aside separately. I then vaped the different crystals and indeed as expected, the majority of the crystals were pure DMT while the other crystals were one of the yellow fractions that I guess got somewhat mixed into the top layer of acetone.




I did TLC on the various fractions but the results seemed to be about the same for all of them, indicating to me that TLC is not helpful for this. I was surprised at how little actual DMT there was in my crystals that looked fairly pure when I first collected them, although it is possible that much of the remaining DMT was hidden inside some of the other layers and just not very noticeable when vaped with those other alkaloids being in abundance.


I also made a video of this process, but not sure it's appropriate to link it here.



In order to pull only these 5 alkaloids from the bark, I did a straigh to base extraction of MHRB using a pound of lye per kilo of bark and pulled with hot heptane, then freeze precipitated the xtals out of the heptane.

If your pH is high (because you used lye), then you can also pull out other very awesome alkaloids from the bark (including one I call MimoLove, which is similar to Metta + NMT), by soaking the bark mix hot in (100F) acetone overnight. Acetone should turn red when it is full of the other alks. Not all MHRB contains MimoLove, however, as a recent batch I tested did not have it. There is an astounding variety of tryptamines in MHRB and it does seem to vary by season. One very cool one I found in one batch produced distinct kaleidoscope visuals for everyone who tried it, and was a very deep, therapeutic experience (LCMS for the kaleido+mimolove stuff here).
moyshekapoyre attached the following image(s):
IMG_20200131_052528_5.jpg (2,572kb) downloaded 266 time(s).
 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
endlessness
#2 Posted : 2/2/2020 2:13:06 PM

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Hey!

Thanks for sharing your experiments!

Didn't you have some TLC equipment there? I'd withhold any judgement regarding your separation until you have confirmation with some sort of analysis like TLC. And it would be very easy to tell you if your supposed separation did work since NMT and DMT separate so neatly. I'd also love for tests on these new mimosa batches you say have more NMT than before.

NMT freebase should be very soluble in acetone like DMT too, so my guess is it did not work as you expect, but I'd still be curious to hear the results of some analysis considering you are so certain from a subjective point of view

Lastly, if you want to separate it in using a proven method, you can try using dry ice.

Be well
 
moyshekapoyre
#3 Posted : 2/2/2020 11:00:14 PM
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Yes, I have TLC here. However, I've now done dozens and dozens of TLC experiments and what I've found is that TLC is basically worthless. I know that sounds retarded, but I've had what looks like almost pure DMT according to TLC which didn't feel like pure DMT, and I've had what felt like pure NMT which TLC shows as mostly DMT. I've confirmed my subjective results with many blinded trials with myself and others. TLC is completely useless in this regard.

I know you're going to say that I'm wrong, TLC right, and that's fine, but all I'm saying is, try the acetone separation. It works perfectly. You'll see.
 
blue.magic
#4 Posted : 2/5/2020 3:35:55 AM

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This looks more like a gradient than "layer separation".

One way to asses your crystals might be melting point determination. DMT has m.p. of 40 °C while NMT has m.p. 87-89 °C.

Another obvious method is TLC. It can be helpful if you have consistent sample volume and concentration, then it may show some difference in amounts of DMT and NMT.

Also a color reagent test on the dilute sample might be useful but since I am not sure if there is some easily available reagent to test NMT specifically, I would use UV-TLC.

If your DMT sample is pure, it should have m.p. close to that of DMT. If the melting point is higher, then there are impurities (not just NMT of course).

Acetone is quite general solvent, it will dissolve both NMT and DMT. The layer you observe miht be just solid particulates from the extraction.

The article "Synthesis of DMT (and analogs) from Tryptamine" on Rhodium archive on Erowid mentions that NMT can be separated from DMT by washing pet ether solution of DMT/NMT with acetic anhydride. Hexane, heptane or naphtha can likely be substitued for pet ether.

Unfortunately, acetic anhydride is a chemical that is hard to obtain (listed precursor), so a home chemist is probably left with recrystallization and chromatography.
 
moyshekapoyre
#5 Posted : 2/5/2020 4:48:40 AM
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Try it out. It works. Smile
 
endlessness
#6 Posted : 2/5/2020 10:46:39 AM

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moyshekapoyre,

You yourself are saying that chromatographical evidence is pointing to something contrary to your own conclusions. I understand you feel the experience difference, subjectively. But there are many other possible explanations that do not involve NMT/DMT separation (for example different DMT polymorphs with different boiling point changing vaporization efficiency and therefore resulting in different effects due to varying dosage).

If you do an experiment, but you already have a pre-determined conclusion that you maintain despite contrary evidence, well, then it isn't a fair scientific assessment.

I understand if you don't want to change your mind, we all can have the opinions we want, but then I suggest every time you talk about such things you avoid talking as if its an absolute truth (for example the title of this thread, or affirmations about NMT/DMT content in mimosa), but rather pose it as a question and/or add clear disclaimers that your conclusions are based strictly on subjective experience but that TLC evidence is not corroborating your conclusions. That way other people can make their own conclusions and decide if they want to repeat your experiments or not, with the full info at hand.
 
moyshekapoyre
#7 Posted : 2/5/2020 11:30:12 AM
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endlessness wrote:
moyshekapoyre,

You yourself are saying that chromatographical evidence is pointing to something contrary to your own conclusions.


No, actually that's not what I'm saying. In fact, the first two TLC tests I did confirmed that there was very little NMT left after doing the above procedure. I didn't mention that, because I tested a few more times and got different results on the same liquid. In the past I've also noticed how variable TLC is, and so I no longer trust it at all to give any type of quantitative info, and sometimes not even qualitative.

It would have been highly dishonest of me to say "I did 2 TLC tests and it shows it's pure DMT" even tho that would have been technically true. Had I not done further tests, I would have probably convinced myself, even, that TLC confirmed my bio-assay findings.

endlessness wrote:

I understand you feel the experience difference, subjectively. But there are many other possible explanations that do not involve NMT/DMT separation (for example different DMT polymorphs with different boiling point changing vaporization efficiency and therefore resulting in different effects due to varying dosage).


I know the difference between a low dose of DMT and a dose of NMT. Furthermore, if I couldn't differentiate those, all I would do is vape some more. Simple.

endlessness wrote:

If you do an experiment, but you already have a pre-determined conclusion that you maintain despite contrary evidence, well, then it isn't a fair scientific assessment.


I did *not* have any belief that this particular separation would be a perfect one. In fact, given my previous attempts with other solvents, I imagined it would be similar in efficiency to the others--a fairly good approach but not perfect. The actual results truly surprised me. I can send you a sample if you'd like to test it with something that is more reliable than TLC.

Speaking of fixed beliefs, it seems that you have them regarding the usefulness of TLC. I appreciate what you have done with spreading these kits around, but I'm simply reporting my observations of their uselessness over here. It is possible that there is some piece of info that's missing. I didn't read that book you linked me to previously on TLC, and I can only imagine that there may be nuances that I know nothing about. If I can find that book I will try to read it and see if there is some explanation of the ridiculous variability in readings. I have spoken with a chemist friend about my issues with TLC, and he simply suggested doing a more rigorous test like GC/MS which he sometimes has access to. I have read that TLC is considered a quick and dirty approach that often saves time, but it is not to be considered conclusive.

Blinded bio-assays actually are valid science, last I checked. So far, I have done a lot of investigation with DMT, NMT and various similar alkaloids, "Metta," "Mimolove," not just on myself, but on dozens of people I know. The results indicate that my subjective perceptions of these alkaloids matches those of most people: NMT alone is not very psychedelic, and too much NMT in the DMT will diminish the psychedelic effect. I'm a good test subject. And I have lots of other willing subjects.

Scientific instruments are wonderful when they work. But human subjectivity is often required to decide whether to take their readings seriously. If it were not for our inherent distrust of instrumentation, we'd all be dead now many times over: https://en.wikipedia.org..._of_nuclear_close_calls


endlessness wrote:

I understand if you don't want to change your mind, we all can have the opinions we want, but then I suggest every time you talk about such things you avoid talking as if its an absolute truth (for example the title of this thread, or affirmations about NMT/DMT content in mimosa), but rather pose it as a question and/or add clear disclaimers that your conclusions are based strictly on subjective experience but that TLC evidence is not corroborating your conclusions. That way other people can make their own conclusions and decide if they want to repeat your experiments or not, with the full info at hand.


TLC is not only not corroborating this particular approach. It is not corroborating anything whatsoever. Have you never seen this happen? Are all of your TLC results actually in agreement with each other? I mean if you test the same vial of something, do you always get the same results on your TLC plate?

As I said, it's quite possible that there is something that I'm doing wrong in my TLC. One thing that I could imagine might be wrong is I don't clean the developing chamber out after each use. Is this a requirement that I've somehow overlooked, perhaps?

In any case, it would be more honest for me to say simply what I said, which is that these are the results I have found based on my blinded bio-assay, rather than to say that these results should be taken with a grain of salt because TLC that is otherwise giving reliable results (it's not) is showing that my bio-assay results might be wrong.

I don't claim anything is absolutely certain. Even if TLC, GC/MS, bio-assay, and NMR tests all agree that this is pure DMT, I still can't be 100% certain that it is. But let's just say at this point, I'm pretty certain. And I think that as more people try this tek, we will get more data that will be more useful than one person doing various tests. After all, I could be just a psycho pathological liar. In which case, I could have said that TLC, GC/MS and so forth all prove this works and I've done every test in the world. So ultimately, it is up to the community to validate this just as it is up to the community to validate every tek.
 
Tony6Strings
#8 Posted : 2/5/2020 1:35:42 PM

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In my experience, dmt can produce vastly different experiences each time it is used. One person smoalking ten times from the same batch of dmt can have ten experiences, each one very different from the other. Maybe what you have come to believe as "metta molecule" is simply good ol spice, producing a different experience than you have come to expect. It is a very interesting substance and cannot be put into a box (although come to think of it I do store my vials in a box of sorts, I stand corrected). It is a ticket to anything, anywhere, any time, everything you can or cannot imagine, aliens, whatever. Its all there on the other side of that pipe.
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You need to hit it with intention to get where you want to be!

"We have arrived at truth, and now we find truth is a mystery- a play of joy, creation, and energy. This is source. This is the mystic touchstone that heals and renews. This is the beginning again. This is entheogenic." -Nicholas Sand
 
Metta-Morpheus
#9 Posted : 2/5/2020 5:16:36 PM

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blue.magic
#10 Posted : 2/5/2020 7:30:38 PM

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You have not ruled out placebo effect. It plays a huge role next to an unknown amount of hidden factors you have not taken into account, for example solid impurities that diluted your sample, removed by centrifuging the vial. This is not separation of DMT/NMT but just purification of the sample, which will of course give you a stronger dose response.

You definitely need to test the product before claiming "Simple perfect separation"

Quote:
It would have been highly dishonest of me to say "I did 2 TLC tests and it shows it's pure DMT"


No it is dishonest to claim it works without doing any sort of analysis.

I hope the community will provide you the "peer-review" Smile
 
moyshekapoyre
#11 Posted : 2/6/2020 10:26:59 AM
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Well, months ago I sent samples off to Benzyme. He hasn't had time to test the stuff. Neither have the other 2 chemists I've sent samples to a long time ago.
So for now, all I'm going on is doing blind bio-assays on many, many people. Despite what y'all might think, that is actually how a lot of scientific studies are done.

Not sure what type of people are here on the nexus who can't tell DMT from NMT from Metta in terms of felt effects, but most people actually can... in fact, I have never in real life come across anyone who could not tell DMT from NMT effects except maybe at a very low dose, and as for metta, most people can definitely tell it is nothing like DMT whatsoever.
Sometimes I feel like I'm in a totally different universe...

Hey Trav, how about we change the name of the DMT-Nexus to be the DMT-(or-Maybe-NMT..Not-Sure)-Nexus...

 
Metta-Morpheus
#12 Posted : 2/6/2020 1:26:39 PM

Fly with the sea birds and sh!t

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moyshekapoyre wrote:

Sometimes I feel like I'm in a totally different universe...



Us too...
“You think that’s air you’re breathing?” -Morpheus
“Whoa fellas, I’m feeling kinda bowling ball-ish.” -Leopold Butters Stoch
It’s got what plants crave. -Brawndo

Magic is here for us all to feel. Naming it isn’t what makes it real.
Running around for us all to know, noticing isn’t what makes it so... -Avett Brothers
 
moyshekapoyre
#13 Posted : 2/7/2020 10:40:25 AM
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Ok guys, new info here plus TLC plates which I need some help to understand... and I'm going to update my OP also.
When you look at the TLC plates, the left 2 plates are from the original purification (DMT, then NMT from right to left, but both show both dots). I guess above a threshold amount of NMT will produce the NMT dot, and vice versa for the DMT, so maybe if there is not enough purity you'll see both dots.

The right 2 plates are the DMT (yellow top layer) from the *double* purified acetone. As you can (barely, sorry) see, those plates have only one dot. I can run more plates but I'm just curious why the dot keeps moving down a little each time. I'm not being super precise with where I pipette the sample, but I don't think I'm anywhere near that imprecise.


When I say I double-purified, what I mean is that I took the DMT that I purified and I re-purified it again using the same procedure as before, but being more careful not to suck up any particles that were sometimes floating in the solution, nor to get too close to the red layer. It turns out it wasn't originally completely pure, but pretty close based on how much NMT I was able to centrifuge out.

Also, what I have found is that the red layer (NMT + dmt) contains a lot more alkaloids apparently than the yellow (DMT) layer. In other words, if I have 5mL of red mix, and I add 10mL of acetone, now I have 4mL of red mix and 11mL of yellow (approximately).

Another thing I've found is that when there is not much red layer left, maybe 1mL in the whole 15mL test tube, if I centrifuge it, it turns into a solid precipitate. I honestly have no idea what the chemistry is behind these results, but I'm very curious to know if anyone can think of anything.

I've realized that a centrifuge is not necessary for this. All you really need is a large test tube, like 100mL or so, and a 15mL pipette that easily fits inside, like maybe 20mL or so. Obviously, using materials compatible with acetone.

I've also realized that the acetone needs to be added to the red layer. Adding the red layer to the acetone doesn't seem to produce a gradient for some reason.. so that should be a hint for anyone trying to figure out the underlying mechanism... or anyone who's by now concluded that I am completely bonkerz. Smile
moyshekapoyre attached the following image(s):
TLC of dmt purification.jpg (1,782kb) downloaded 132 time(s).
 
endlessness
#14 Posted : 2/7/2020 1:02:22 PM

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There doesnt seem to be much difference between the first and the second plates apart from concentration, so it doesn't seem to indicate you are separating out the NMT.

Instead of using a pipette, you want to use a microcapillary tube, you'll have a much better resolution of the spot. Load just 3 or so microliters of the dissolved sample, slowly adding to the plate so its evapping as you load, and this way it concentrates in the middle instead of loading a more diluted larger circumference circle on the plate.

As for the right two plates, it seems they are significantly less concentrated than the left ones, so it's hard to know if indeed there is no NMT or you just made it so diluted that you cant see it. Also, using the capillary you can compare at least two or three samples per plate, running them side by side is much better to compare than running different plates per sample.

Also, in order to have a better comparison, it would be more accurate to actually control the concentration of your samples, so first dry the samples, then dissolve the same amount of each in the same amount of solvent that you'll use to load the plate with a microcapillary.

Are you waiting for the eluent to reach the top of the plate the same each time? You def should if not. What eluent are you using, the methanol:ammonia mix?

Thanks for sharing the result of your research!
 
moyshekapoyre
#15 Posted : 2/8/2020 12:27:50 PM
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endlessness wrote:
There doesnt seem to be much difference between the first and the second plates apart from concentration, so it doesn't seem to indicate you are separating out the NMT.


Right, that's why I say that TLC is not very quantitative, because the felt effects between the stuff on plate 1 and plate 2 are tremendously different, with plate 2 not being psychedelic. As a reminder, those first 2 plates were produced using alcohol to separate the DMT + NMT, which is not nearly as efficient as acetone.


endlessness wrote:

Instead of using a pipette, you want to use a microcapillary tube, you'll have a much better resolution of the spot. Load just 3 or so microliters of the dissolved sample, slowly adding to the plate so its evapping as you load, and this way it concentrates in the middle instead of loading a more diluted larger circumference circle on the plate.



Sorry, I meant microcapillary tube when I said pipette. Didn't have the vocab (and for some reason I'm already forgetting that term).

endlessness wrote:

As for the right two plates, it seems they are significantly less concentrated than the left ones, so it's hard to know if indeed there is no NMT or you just made it so diluted that you cant see it. Also, using the capillary you can compare at least two or three samples per plate, running them side by side is much better to compare than running different plates per sample.


Ah, ok, I see, so there is some nuance I wasn't aware of then. I didn't know that if the sample is not large enough, it could change the ratios and even eliminate one of the substances from the results. I'm starting to understand why my results have been so unreliable. Thank you.


endlessness wrote:

Also, in order to have a better comparison, it would be more accurate to actually control the concentration of your samples, so first dry the samples, then dissolve the same amount of each in the same amount of solvent that you'll use to load the plate with a microcapillary.


Perfect, thank you for the extra instructions. I've done that now. Photo attached. Little blurry so let me explain. On the left is my purified DMT (clearly I didn't do a perfect job, but it does look pretty good, and I'm sure I could have done it more carefully).
Next is some stuff that I had lying around which felt very much like NMT with no psychedelic effect. It looks on the TLC like it has a bunch of DMT as well.
So there are 2 explanations:
1) NMT does not dissolve easily in the eluent. So whatever little DMT is in there dissolves more favorably, leaving a disproportionately large spot to what is truly present in the sample. I'm attaching another photo to show how the NMT does not like to dissolve in the eluent. I have to shake and prod and shake and prod to get NMT to dissolve, and even then it doesn't dissolve fully, whereas DMT dissolves very quickly. You can't see the NMT that was really hard to dissolve in the mixed vial, because I did manage to fully dissolve that after a while of shaking & prodding, possibly because it already in an oily form rather than fully solid.
2) It does not have to be pure NMT to feel just like only NMT, because NMT apparently has a higher receptor binding affinity.
The third dot is DMT+NMT that I have not even vaped yet to see how it feels, but just extracted. In any case, what I'm saying is that TLC does seem capable of telling you if your DMT is pure enough to not feel NMT effects, but it does not seem capable of telling you if your DMT is so full of NMT that you won't feel DMT effects.

endlessness wrote:

Are you waiting for the eluent to reach the top of the plate the same each time? You def should if not. What eluent are you using, the methanol:ammonia mix?

Thanks for sharing the result of your research!


I feel the results of my research are worthless if they are not spread for the benefit of others.

Now that you mention letting the eluent reach the top, as you can see, I didn't do that on the last plate, so that explains why that dot was lower, I guess.

I usually leave the plates in the developing chamber for way longer than necessary (because I forget). I assume this is no problem.

The eluent is just whatever comes in the BunkPolice kit. I guess that is methanol:ammonia? It doesn't say, but it sure does smell like ammonia. For some reason they seem to make it sound much more toxic than methanol:ammonia tho. Like, it's not all that dangerous if some methanol:ammonia touches my skin, right?
moyshekapoyre attached the following image(s):
dmt purificaton acetone success.jpg (1,686kb) downloaded 101 time(s).
nmt not dissolving well in methanol ammonia.jpg (3,091kb) downloaded 99 time(s).
 
 
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