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DIY TLC plates

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grollum

grollum

Rising Star
I am just reading into the possibilities of separating 5-MeO-DMT and nn-DMT. Sofar i think the TLC plate separation is the way to go. Do I understand this right? You need maybe a bigger plate depending on the amount of freebase. Then after spotting and developing your dmt mix you need to scrape it of the plate in which height is needed for one or the other and then separate again from the silica and other stuff?

Is this somehow right?

I also found this DIY tec to do plates by your self:


Anyone tested this or another method?
 
How do you know you have a mix of 5-MeO-DMT and DMT in the first place?

TLC separation is possible, though generally you'd need to make preparative TLC because normal TLC plates might be too thin and you wont be separating much material in the first place.

Also another question is, how will you visualize the spots? If you use comercial TLC plates, they generally will have a UV fluorescence indicator, so with a simple short-wave UV light you can see the spots and know where to scrape, but if you're preparing TLC yourself, the normal silica wont have the UV fluorescent indicator. You'll need some reagent to show the spots and know where to scrape the silica, but a reagent generally will destroy the sample, so you need something else. While they definitely exist, I'm unfamiliar with non-destructive TLC visualization methods apart from UV light with the plates I mentioned, maybe a chemist here can help.

Another option is to use column chromatography for separation and use TLC just to check your separation, so in that case you'll be able to use a destructive reagent for visualization if you dont have the UV fluorescent plates. If you want the UV fluorescent plates, click my signature for more info on TLC kits, might make things simpler for you.

As for the eluent, I've been using methanol:25% ammonia (100:2.5) for general tests and it does separate 5-meo-dmt and dmt but the separation isn't the best. According to literature you could also try the following eluents:

2N acetic acid
Rf
DMT 0.50
5-MeO-DMT 0.60
(Dutta & Ghosal 1967)

or

t-Butanol-acetic acid-water (70:2:29)
Rf
DMT 0.50
5-MeO-DMT 0.40
(Duttha & Ghosal 1967)



Another way of separating them is through solubilities. One possibility is by the solubility of the acetate salts in chloroform, as you can read here. It might work with other solvents appart from chloroform, might be worth a try. If you use chlorinated solvents please dont leave the alkaloids for too long otherwise they might react.

Yet another option that was once discussed but unconfirmed if it really works is by the solubility of the citrate salts in acetone. Might be worth a try.

That being said, I still wonder how you think you have that mixture in the first place.

Lastly, please do share whatever are the results of your experiment if you go ahead with this, we could all learn from it for sure :)
 
If I understand correctly (any chemist please correct me if Im wrong), N= normal solutions, which means 1 gram equivalent weight of the substance in each 1000 mL of solution. So 2N = 2grams/liter

So wolphram alpha says 1ml acetic acid = 1.05grams.

If 1.05g = 1ml, then 2g = X ml

x = 2*1 / 1.05

x = 1.9ml

So for to make 1l of that eluent, you need 1.9ml glacial acetic acid + 998.1ml water.
 
endlessness said:
any chemist please correct me if Im wrong
Click to expand...
OK :)

Equivalent concentration - Wikipedia

en.wikipedia.org en.wikipedia.org

In chemistry, the equivalent concentration or normality of a solution is defined as the molar concentration ci divided by an equivalence factor feq:

Normality = ci/feq
Click to expand...

For acetic acid the feq is 1, so a 2N solution of acetic acid contains 2x60 = 120g/L, as the Mw of acetic acid is about 60. You can repeat the calculation above using 120 instead of 2 to find the required volume of acetic acid to make up a 2N (==2M - in this case) solution, or just weigh out 120g of acetic acid and make it up to 1L in a suitable (volumetric) flask.

Note that this equates to a 12% solution, so normal vinegar is not suitable for this preparation. If you're fortunate to be living somewhere where 25% acetic acid vinegar concentrate is available in the supermarkets then this product can simply be diluted in an equal amount of water to make the 2N acetic acid solution, to a reasonable approximation.

1 gram equivalent weight
Click to expand...
this should be "1 gram-molecule equivalent weight". Then it all works properly.
 
@endlessness:

I think I might have a mix of both because the sources I like to use are known to have both in it.
Like Phalaris spp. and Acacia simplex for example.

I could imagine to visualize the spots once to get the position and then measure that position on other plates. Or is this not possible because of variation?

You think this UV fluor feature cant be done DIY? Will google this down!
Thanks for the eluent infos. That helps a lot!

I have to wrap my head around column chromatography.

Did you try out the acetate chloroform tec? I am wondering in what category hordenine and gramine would fall.

It sounds really great.

I saw the acetone tech and was wondering why the hell the results are so different each time. Maybe temperature?

Will wrap my head first around the acetate chloroform tex and then see further… Thanks a lot!
 
grollum.

I just recently sent some acacia simplex extract from another user and it only had dmt. Still waiting for the mass spectra files to see if there are other smaller peaks they didnt care to mention. What source says that it has 5-meo?

You're right some Phalaris has 5-meo but it depends on the species and variety. Are you considering wild extraction or growing a known specific clone for example? Did you already try this extraction or still planning it?

I think it could be possible to visualize the spots and repeat and "guess" where they are in the next plate, as long as all other conditions remain equal, like doing it one after the other without taking too long in between. If you do it on different days or places with different temperature, humidity etc, then it can vary quite a lot.

Also you could take a small sample of the separated fraction and re-do the TLC but using a destructive visualizing reagent to see if the separation worked.

Im not sure if the UV fluorescence can be added at home to the homemade silica tlc plates, let me know if you find out.

I personally never tried the acetate tek, no.

Good luck!
 
endlessness,

it seems that I had this wrong in mind. Could not find any source which mentioned 5-meo.
I am curious now what results the spectra brings forward. And how much nmt will be there.
Do you know the used tech?

I am planing to extract from clones (big medicine and AQ1) as well as brachystachys.
But I don't know the trustworthiness of the clones. Will have to TLC that first. If its quite clean all is good!

No news on finding info's on DIY UV fluorescence TLC plates.

Will let you now when things get concrete!
 
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