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benzyme
#1 Posted : 8/21/2018 2:55:18 PM

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As I've mentioned, I got my CombiFlash Rf back, after lending it to a biohacking company for a few months. I've ordered a new deuterium lamp, and will install it this week. Depending on demand, I'm considering offering a new service: flash purification of otherwise difficult-to-resolve analytes. The service would essentially provide reference standard-quality products. I'm thinking starting price will be $30 per analyte (mg's of sample...larger samples will have a higher price), as it's not expensive to run. This would mainly benefit those who run TLC, but need preparative scale purification, or those who can't resolve resinous materials. It can also extract from raw material, and yield >99% pure product. I have columns that can handle anywhere from 4.3 mg to 22 g of sample.

Mods, let me know if this is out of the scope of Nexus rules, and I'll delete it.

here is a primer on purification by liquid chromatography.
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endlessness
#2 Posted : 8/21/2018 3:07:20 PM

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Sounds awesome Benz Smile

We should prob collaborate when we get plant samples that have unknown compounds, separate them with flash chromatography and then try to id them with different methods, maybe sending it to someone with NMR if our other methods aren't enough.
 
benzyme
#3 Posted : 8/21/2018 3:10:40 PM

bioanalytical chemist

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great idea.
I'm also going to follow the TLC group more closely, as the translation from TLC to flash is pretty straightforward.

also keep in mind, the larger scope of this...to prep reference standards that would be otherwise difficult/expensive to source, and standard curves can be prepared from them, to generate quantitative data, i.e. potency
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of knowledge at our disposal. The rest is poetry, imagination." -Max Planck
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burnt
#4 Posted : 8/23/2018 4:21:36 AM
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Nothing really to contribute except want to say that flash chromatography is awesome and I feel column / flash / prep chromatography is the next phase for the DIY chemist community. So glad to see someone taking initiative. I love nothing more then starting with TLC, going to column, optimizing method, and then cranking through lots of runs to get pure compounds.

For those interested I'd recommend two books to learn:

Advanced practical organic chemistry:

https://www.amazon.com/A...tical+organic+chemistry

Love that book

And Experimental Organic Chemistry:

https://www.amazon.com/E...icroscale/dp/0632048190

Great resources.
 
blue.magic
#5 Posted : 8/23/2018 11:59:01 AM

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burnt wrote:
For those interested I'd recommend two books to learn


Thanks. I got this one so far:

Applied Thin-Layer Chromatography: Best Practice and Avoidance of Mistakes

 
Questfinder
#6 Posted : 8/28/2018 5:54:30 PM

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Purified via preparative chromatography would an extract be suitable for intravenous use?
 
endlessness
#7 Posted : 8/28/2018 9:47:11 PM

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There are other issues with IVing apart from the DMT purity itself, though that's certainly one of the main concerns. We have talked about it in other threads, check this FAQ entry

https://wiki.dmt-nexus.me/FAQ#Can_DMT_be_IVed.3F

Chromatography might certainly clean some impurities, if you choose well the mobile phase and the stationary phase... Though you'd also have to be careful with the quality of the eluents you use because you dont want to leave traces of impure eluents after having cleaned the DMT of other things.

As the link above says, I wouldn't recommend it, but if you do it, please take the precautions mentioned there.
 
Questfinder
#8 Posted : 8/29/2018 5:05:53 AM

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Thanks Endlessness, I knew there was topics on the subject already so perhaps I should have re-read them before asking my question.

Purity is still my only concern personally. I'll stop beating around the bush: would synthesized DMT be any more suitable than extracted? For a long time I had always believed it would be, but now that I understand the chemistry a bit better I'm really not very sure, the potential impurities in a synth, though fewer, would appear to be much more harmful. Seems to me multiple purification steps need to be undergone and sterile procedures followed regardless of the route taken. What are your thoughts on this?

Hope I've not taken this too far off topic Pleased
 
endlessness
#9 Posted : 8/29/2018 7:00:41 AM

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Per se, no source is better than the other, it's all about the purity of the compound, which will depend on what chemicals you use and their purity, as well as how well you perform the extraction and clean up steps. Def multiple purification either way is important.
 
Questfinder
#10 Posted : 8/29/2018 7:28:41 AM

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I had suspected as much, but it's good to have the opinion of someone such as yourself Smile

Many thanks.
 
downwardsfromzero
#11 Posted : 11/30/2018 6:53:31 PM

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Another thread I missed last summer...

It seems worth throwing in here - dry flash chromatography is a simple and handy preparative tool within reach of the home chemical hobbyist. It even lends itself well to solvent gradient separations.

One of these days I'll get mine set up.
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