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Identifying LSD through NMR spectra

Z

Zastavok

Greenlighter
Joined
Jul 17, 2010
Messages
2
Hey guys,

So basically I have access to a 600 MHz NMR spectrometer. I was wondering if it'd be easiest to just run a simple 1H proton scan on any batches of L that come my way to identify whether or not it is actually the compound advertised. I think this would be simpler than buying a test kit seeing as I'd be able to simply run a scan and have the spectra within ten minutes. It would also be possible to easily determine what the compound was if it were something other than LSD-25.

If anyone has experience with this I'd appreciate. I was thinking of dissolving say a tab in say CDCl3 to let the LSD come out from the blotter paper and then running a scan. Would other solvents be better suited such as an ethyl acetate mix or maybe DCM? Also would any of these solvents react with the LSD if I were to combine.

Any help/input is appreciated.

Thanks.
 
I doubt you can get a good proton from 0.1mg of something in ten minutes, even if you have a 600. You'll probably just see solvent.

If you have access to NMR, you probably know how to do TLC as well. Assuming that you have an authentic sample, that might work better. Plus, you can do it at home.
 
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Extract blotters with cold deuterated methanol overnight in the dark, then run on NMR. LSD tartrate (the water soluble salt of LSD we all know and love) is not soluble in chloroform, and doing acid/base extractions is a good way to destroy your LSD entirely. Minimal sample manipulation is what you need.

The SWGDRUG paper on this has more info on sample prep.
 
Yeah, another analytical method like TLC might work better, or mass spec. Even on a 600 with 1 mg sample it usually takes a few hours worth of scans to see *anything*. If you decide on NMR, see what probe the spectrometer has - if it has a cryoprobe you can actually get a decent proton spectrum with an overnight run for a 1 mg sample.
 
Ethyl_Acetate said:
Yeah, another analytical method like TLC might work better, or mass spec. Even on a 600 with 1 mg sample it usually takes a few hours worth of scans to see *anything*. If you decide on NMR, see what probe the spectrometer has - if it has a cryoprobe you can actually get a decent proton spectrum with an overnight run for a 1 mg sample.
Click to expand...

I don't know what NMR you are using, but on a 400 I routinely can get an adequate 1D proton spectrum with 16 scans on 1 mg of compound. This is using presaturation for water suppression without a cryoprobe.
 
tryp2fun said:
I don't know what NMR you are using, but on a 400 I routinely can get an adequate 1D proton spectrum with 16 scans on 1 mg of compound.
Click to expand...

I don't remember specifically what 400 MHz machines or probes I was able to use, unfortunately. Good to know there are some that can generate quality spectra. Regardless, as long as you can generate a spectrum with clean splitting and decent integrations you're set, and assuming you can recover your sample you could give it a shot.
 
Zastavok said:
Hey guys,

So basically I have access to a 600 MHz NMR spectrometer. I was wondering if it'd be easiest to just run a simple 1H proton scan on any batches of L that come my way to identify whether or not it is actually the compound advertised. I think this would be simpler than buying a test kit seeing as I'd be able to simply run a scan and have the spectra within ten minutes. It would also be possible to easily determine what the compound was if it were something other than LSD-25.

If anyone has experience with this I'd appreciate. I was thinking of dissolving say a tab in say CDCl3 to let the LSD come out from the blotter paper and then running a scan. Would other solvents be better suited such as an ethyl acetate mix or maybe DCM? Also would any of these solvents react with the LSD if I were to combine.

Any help/input is appreciated.

Thanks.
Click to expand...

I ran NMR spectra for 4 years. You need mg range quantities, although I imagine the tech has advanced somewhat since I last used this.

CDCL3 would be a good solvent IMO.

Tom
 
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