First steps with Chromatography

[benzyme]

yes.

I've differentiated between psilocin and psilocybin using tryptamine hcl standard on whatman paper, @ 365 nm.

having both lights available is handy, just be careful with 254, don't leave it on for long periods of time near plastics or rubber. it induces crosslinking in polymers, rubber, and DNA.

 

[Tannenberg]

yes.

I've differentiated between psilocin and psilocybin using tryptamine hcl standard on whatman paper, @ 365 nm.

having both lights available is handy, just be careful with 254, don't leave it on for long periods of time near plastics or rubber. it induces crosslinking in polymers, rubber, and DNA.

i know the hazzards that come with UVC lights. I would shield the bulb and only light the sample if i ever get one.

Whatman paper, that "grade 1 chromatography paper" that is pretty cheap and comes on 100m rolls?
Will it work great for DMT analysis in plants / grass? Or would you recommend to buy silica plates for that purpose?

 

[benzyme]

doesn't really matter, because the functional groups in both stationary phases have similar intermolecular forces involved. what matters is the selection of solvents.
the mixture I listed would work particularly well, it's listed in a couple books I've posted in advanced chem.

 

[Tannenberg]

doesn't really matter, because the functional groups in both stationary phases have similar intermolecular forces involved. what matters is the selection of solvents.
the mixture I listed would work particularly well, it's listed in a couple books I've posted in advanced chem.

so you mean "butanol, EtOAc, NH4OH. 4.5:3:1.5"?
endlessness said something about 100:2.5 ethanol / amonia, i think i will try this first, because ethanol / ammonium hydroxide is pretty easy to get.

edit: if i got 10% amonium hydroxide solution, do i have to use 75:25 ethanol / 10% amonium hydroxide? I think this is pretty contra productive, is i don´t want 2.5:22.5:75 amonia, H2O, Ethanol?! Or can´t i use amonium hydroxide and have to bubble amonia through ethanol?

Thanks for your help!

 

[endlessness]

I think saturated ammonium hydroxide is around 35%, which is whats added to the ethanol. The ethanol used was already 96%. The extra water content might affect a bit the polarity and hence the Rfs, but it should work, try it out by raising equivalently the dilute ammonia, then try again adding a bit less and see how spots look etc. Let us know!

 

[benzyme]

..from The Alkaloids - Plant Analysis and Substance Testing - Welcome to the DMT-Nexus

yeah, son. I've prepared p-DMAB-TS, aka Van Urk's reagent, several times (for ergine characterization) at home.

 

[Tannenberg]

Whats the main difference between Van Urk's reagent und Ehrlichs? I mean both use p–dimethylaminobenzaldehyde and Van Urk´s only has ethanol added. I am correct?

B.t.w. i managed to get some 9% Amonium Hydroxid and some 96% Bio-Ethanol. 1 liter each.
I hope it will work with 9%.
The Ethanol also contains 1% of Butanone and bitrex (tax reasons..) i don´t know, maybe this will become a problem too (i think the butanon may move at a different speed in the static phase).

I will try it in the next days, because i don´t want to use glasses i use for drinking / eating. I well get some borosilicat glasware (i already have it, but i have to pick it up somewhere else).

 

[endlessness]

Ferric chloride is the difference in Van Urk / PDMAB-TS, has some bit different color reactions.

I bet your solvent mix will work but the Rf's will be different than the system I used. In any case if you can extract some DMT from mimosa, you'll see the main spot being DMT (maybe another small spot being NMT, possibly another for 2mthbc too), so you can use that as your "standard" to compare against other potential dmt-containing plants.

Dont forget to take pics of the tests and show us.

 

[Tannenberg]

i will try it and as soon as i get some results post it here

I found a local lab supplier here (online store) which has pretty cheap whatman chromatography paper (15€ / 1cm / 100m roll), i think i will order there. They also ship to "normal persons".
But i have a company since 2005, maybe that should help getting some stuff but don´t know how much they ask what i am doing (i mainly do programming, no chemistry)..
They also sell spray bottles for reagents b.t.w.

I don´t have mimosa but maybe i find a seller that sells small quantities of it so i can use it just for comparision.

Another thing, i don´t know who manages this forum here, but maybe he / she should get a ssl certificate from startssl.com because they are for free and don´t cost 49$/year (accepted in all big browser b.t.w.).

 

[benzyme]

Ferric chloride is the difference in Van Urk / PDMAB-TS

van urk's doesn't always have ferric chloride, there are various formulations.

 

[endlessness]

Tannenberg, can you pm me the web address of this company? What kind of spray bottles is it, and how much does it cost?

Benz, sorry I misunderstood you in the chat, I thought you had said van urk = PDMAB-TS

 

[benzyme]

no worries

there are various 'recipes', using 1 or 2% of p-DMAB in acidic alcohol (ex. 10 mL sulfuric or hydrochloric acid in 90 ml 95% ethanol), with or without FeCl2. the subsequent treatment with Dragendorff's reagent is what supposedly enhances visualization

here is a fairly interesting blog on classic LSD research, with reference to the reagents

 

[endlessness]

you think acetic acid/vinegar would work as the proton donor? Wondering how "kitchen chemistry" this can go, considering p-DMAB and FeCl2 can be sent dry to others.

 

[benzyme]

tbh, I'm not sure. definitely worth a try.
I don't see why it wouldn't work, the purpose of the acid is to protonate the adduct so it forms a complex with the pyrrole carbon at the 2-position of indole