DIY Thin Layer Chromatography

[benzyme]

whether one is extracting alkaloids from seeds or plant material, it helps to have a means of analysis, and a reference to compare it against. attached are a tutorial to make your own TLC plates, and a chapter on alkaloids from 'Plant Drug Analysis-A Thin Layer Chromatography Atlas'

 

[actualfactual]

good info. thanks.

 

[Infundibulum]

Amazing stuff!

This is great for someone who wishes to test their local flora for dmt.

 

[Adivino]

In case one wanted to get the book, where was the second pdf taken from?

 

[benzyme]

http://ebooklink.net/g/download/3540586768/Plant%20Drug%20Analysis:%20A%20Thin%20Layer%20Chromatography%20Atlas/

 

[benzyme]

bam.

 

[Shaolin]

Erowid - for 5-MEO but a nice overview.

Also Wizard-X to the rescue. X-file 7.

 

[The Traveler]

I see in this place that you can buy a roll of 1" x 100yd of Chromatography paper (you need about 8 inch of paper per test, so 450 tests on this roll) for only USD 25,75: click!

Benzyme also told me in the chat that you need:
* ethyl acetate and methanol (or ethanol/IPA instead of methanol) as the Eluent, the solvent being used to push the mixture
* UV light at about 300nm
* pipet or eye dropper to make the tiny droplet on the paper
* A jar that can be closed as the 'reagent chamber'
* Preferable also a reagent spray (it's not really needed but it can make the results more clear)

Also I like to point out that TLC is a qualitative and not quantitative measurement. So it gives you the relative abundance info, qualitatively. It's not to measure the percentages of the different contents.


Kind regards,

The Traveler

 

[benzyme]

yes

this is good stuff.
the implication is simple, folks: the future availability of root bark is questionable.

it seems like a good time to look at other plant sources. TLC/paper chrom are easy methods of
characterizing the different alkaloids. once one gets the hang of this method, column chromatography is the next step...sample preparation.
the diagram posted by Shaolin is a good one. it's vacuum column chromatography.

 

[Shaolin]

The Home Scientist 024 - Making thin-layer chromatography (TLC) plates

[YOUTUBE]

 

[burnt]

While I'd certainly encourage do it yourself TLC just one note. Silica dust is toxic. It will get in your body and stay there. Its kind of like breathing asbestos. So just make sure to wear mask when making your own TLC plates or cutting up TLC plates. Also work in an area you can easily clean etc usual lab stuff.

 

[Aegle]

Benzyme

Nice this thread is awesome, shot a lot. 8)


Much Peace and Rainbows

 

[ragabr]

SWIM is planning on starting up a bunch of Illinois Bundleflower seeds, and was hoping to use this to determine which plants to save seeds from. It looks like the only appropriate method given in 'Plant Drug Analysis-A Thin Layer Chromatography Atlas' is method C, but I don't think di-ethyl ether will be easily available to her.

Does this even seem like a reasonable approach, and might there be a more readily available substitute for the ether?

 

[benzyme]

it's roughly 60/40 ether/heptane

 

[rOm]

Thanks a lot for the infos BEnz and al.

 

[Dr_Sister]

Yes, very informative thread!

Question: To visualize dmt or yuremamine would a UV light be sufficient or would a stain of some sort be required? If a stain is required, would iodine vapour or vanillin/EtoH/H2SO4 or perhaps even dilute H2SO4 stains work for this?

Thanks
Sister

 

[benzyme]

Ehrlich's reagent (aka Van Urk's) is a qualitative test for the presence of indole alkaloids; the azide complex it forms results in a characteristic color for each respective alkaloid.

it is p-dimethylaminobenzaldehyde in either 2% H2SO4 or HCl.

Siser, i'm sure you've seen this, but in case you haven't, here.

 

[Dr_Sister]

Siser, i'm sure you've seen this, but in case you haven't, here.

No, I'd overlooked that Benzyme. Thank you.

 

[Dr_Sister]

Well, after several attempts Sister has something that is getting close, but no cigar yet.

Ehrlich's reagent is working fine, although it needs some heat to develop fully.

Initially sister was getting huge blobs as results, but after diluting the product and switching micropipettes Sister is now getting thin streaks, very consistently. When product is diluted even further she gets no results, so Sister thinks overloading the sample is not the problem.

Would adding some NH4OH help with this streaking problem? The anticipated product being largely amines.

Also the rf for the top of the streak (also darkest spot in the streak) is like rf 0.9, so sister is wondering if a less polar eluent might be called for? She has been using EtAcO/MeoH - 3:1

Has anyone else encountered this issue? And if so, how did they work around?

Thanks
Sister

 

[Dr_Sister]

One other question about Ehrlich's reagent. Sister has been trying it on other compounds as well and notices slightly different colours depending on what amine is spotted. The colours range from teal to blue to purple. Is there any way the colour of the spot can be used to determine some of the characteristics of the compound being spotted?

For instance would a primary or secondary amine give a different colour result than a tertiary or saturated amine? Would a beta-carboline give a different colour from an uncyclized amine?

This is a long shot, but is anyone aware of the existence of a colour chart to interpret these results? Any refernces would be greatly appreciated.

Thanks again
Sister