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Poor man's Column Chromatography for Phalaris

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anonhippie

anonhippie

Rising Star
This might be too advanced for me, but I really want to keep trying phalaris. I really don't want 5meoDMT however, so I've decided that if I'm going to insist on phalaris then column chromatography is the only way to go.

Starting Material
So lets say I've done the hippie salad tek correctly on phalaris aquatica. I should have a goo that contains DMT and 5meoDMT. I can redissolve this in acidified water.

Mobile phase/Eluent
I've read here that I can use acetic acid as a solvent, in the preparation of my eluent. I don't have acetic acid right now, unless I were to use vinegar (and even then the vinegar I have isn't white distilled vinegar). I have citric acid, would that work? I've also read of people doing TLC using a mixture of ethanol and acetic acid here. So I suppose that might be better than just plain acetic acid. I'm really hoping I could use citric acid with ethanol.

Stationary Phase
The stationary phase is more difficult.
* I could buy silica gel as white, untreated desiccant. Its the cheapest option for me right now, I'm not in the US nor the UK and I can't easily buy the ~50um silica gel. I can buy those big beads of silica gel used as a desiccant though and then I could grind it up as mentioned here:. To grind that much silica gel for column chromatography would be very difficult and time consuming with my equipment on hand however.

* What if I used cotton? Sounds crazy but apparently people used cellulose powder before. Cotton isn't too different from that...

* Paper also works in TLC, why not column chromatography?

With both these last materials I could cut them up as much as possible to increase surface area while increasing flow rate.

Equipment
The column doesn't have to be complicated right? I could take a long but thin glass bottle, there are plenty of those around me in the form of limoncello. I could cut off the bottom by scratching a ring around it, and then hitting it against the wall. I could block off the neck and make a nice little stream come out by using those lovely inserts they make for all sorts of alcoholic bottles so that they don't spill when poured quickly into cocktail galsses. I'd probably add some kind of screen and some sand too.

I then invert it, stuff it with cotton/paper/silica gel, and then pour my eluent down there.

If the eluent doesn't flow, I could jam the neck of the bottle into my vacuum-filter beaker, somehow sealing it, and then pump it through, doing a "flash column chromatography"

Process
So assuming I get these materials together and run my extraction through it, I could take fractions that would be water with unknown compounds. I could then run a TLC on each sample, and use a party-light 365nm (source) UV to detect which had the DMT. Then I would run the hippie salad tek on that sample.

Then I should have more or less pure dmt.
Or a lot of wasted time...

Suggestions?
 
Ah, I think that is what I was talking about as a possibility with my setup.

You mean like this, right? http://www.erowid.org/archive/rhodium/chemistry/equipment/dry-column.vacuum.chromatography.html


Looks like I'll have to come up with some kind of adapter to avoid the problem of disassembly... brass fittings will be easier than glass here.

Any idea on using cellulose rather than silica? Does a mixture of citric acid with ethanol provide a viable solvent, or is there something inherently wrong with that?
 
I don't think cellulose is going to work as well as sillica. You could try it and report back.


Also citric acid and ethanol doesn't sound too good either. Check solvent systems with TLC, it's a complimentary technique to column chrom. I see no reason why brass would be better then glass at all. Not sure what the problem of disassembly is either.

Unfortunately no one can look at a lot of solvent combinations and out-right say "That won't work", unless its really obvious. Ethanol and citric acid to me sounds like it wouldn't work at all. It's an experimental science. If you can't spend 30 bucks to experiment to find a cheap way to go about it, chances are you'll have to wait for someone else too. So far, not too many people have even tried for that reason.

Keep in mind.
A little work-up time saves a lot of TLC time.
A little TLC time saves hours of column time.
 
Thanks InMotion for the advice, I've done a little more research on the internet I've found no one mentioning using citiric acid with any kind of chromatography with organic chemistry.... silly of me to hope that anyway.

I'll see what I can do given that I'm in Italy right now and I don't want to spend a lot of money getting things shipped to me; I'll report back on any results.

(The brass was just for practicality to make an adapter as shown in that link above for vacumn chromatography... its good to at least hear it won't cause any harm)
 
Hello everyone, I am just a noobie, so correct me if I am wrong. I was thinking how to separate NN - DMT from the mixture of alkaloids you get while extracting from Phalaris. I checked couple of forums yesterday and the method, that seemed quite useful was sublimation at certain temperature (wiki varies from 83 - 160 degrees of Celsius). The sublimation temp of NN - DMT is much more lower than the temp of other alkaloids (5 Meo DMT, Hornedine, Gramine), so it could purify the final product. What do you think about it?
 
Donnie the sublimation point of dmt is not known, let alone how to seperate from other alkaloids in that way. Vacuum or column chromatography coupled with tlc would be your best bet in that situation.
 
AH, I'm all for cheap science, but I think you're trying to go a little too ghetto here.

Glass tubes are cheap, and so is silica. Probably the cheapest OTC source is silica cat litter.

Grinding and sieving the silica should be pretty easy and cheap also. Anything from a coffee grinder, blender, or mortar and pestle should work just fine.

You won't need a vacuum or pump. You should only really need that if you use ultra fine silica, otherwise it will be much easier to just wait for it to run.

You really need to replicate a proven procedure first. Since it doesn't sound like you'll take that advice... you at least need to change only one thing at a time from proven procedures. Otherwise you're going to end up with a total failure and no idea why. (ask me how I know ;)

I would not try cotton or DE. Cotton just sounds like a bad idea, and IIRC DE is just used as a support and probably won't interact on it's own.

Good luck, and keep thinking. But do yourself a favor and only try one crazy idea at a time.


-FF
 
Why not simply doing naphtha pulls? My tests showed its pretty selective for DMT and not for gramine/hordenine. Do a TLC after to make sure you have what you want, and thats it...

If you want to play with column chromatography, it's fine, I give all the support, but you can also try the easier way before.

By the way, one can also use preparative TLC for separating substances.
 
I think paper might be a pretty easy route. Roll up some paper in a tube, run your product, cut out the right band and extract from it.

Couldn't get much easier than that.
 
In my experience, naphtha pulls very little to nothing from the grass. I don't know if the dmt is present in oxide form or what, but naphtha doesn't seem to pull it for one reason or another.

I suspect if you want to use naphtha for grass extraction, a zinc reduction such as that in the On Processing Phalaris PDF may be in order.
 
Hi everyone, thanks for the advice. I've decided to not use phalaris in the near future, as I've obtained enough MHRB to keep me busy. For anyone that wants to try this, it sounds like fastfred's idea of using silica cat litter would work well.
 
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