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The Mescaline Extraction Thread

Migrated topic.
If precipitating hcl crystals out of solution you require very fine filter paper most likely, as they pass right through Whatman grade #1 filter papers. #1 filter paper and coffee filters are fine for filtering scraped up hcl crystals from an evaporated salting, though SWIM usually just decants away the liquid. Hope this helps.
 
Ello all,

I'm trying to decide which way to go about extracting cacti. I don't have access to toulene but I can get MEK and xylene. For acids I can get vinegar, citric acid and I'm guessing HCL but I believe the fumes from HCL are harmful? Was thinking of adding cacti to water with a splash of vinegar and doing a few pulls like that (essectially like making tea) and then reducing and filtering, then basing with sodium hydroxide (don't think mescaline is sensitive to high PH) and then pulling a few times and either salting with vinegar (but it looks like acetic mescaline is hard to handle) or citric acid ( don't knowmuch about that).

This will also be to test a cacti's relative potency as I don't plan on seperating the mescaline fromother alkaloids.

Any and all comments or advice much appreciated; thanks. <3
 
It seems you're going in the right direction.

Few things :
A good tek is Kash's A/B Mescaline Extraction

First step, Freeze&thaw the fresh cactus or the hydrated powder (or chips). I prefer chips (dry or fresh cacus cut in small bits) as it's easier to filter compared to powder (or fresh crushed) and it seems there's not mescaline left after extraction.

Second step, A pressure cooker is very efficient to water extract (3x30min). It saves lots of time compared to boil in a pan. Warning, first boil, be sure to boil with no cover until it doesn't foam anymore otherwise it could clog the pressure release valve (or repaint your kitchen)

I prefer to filter before reducing and you can decant after reducing but the mud leftover still contain mescaline so i extract from this mud.

Xylene (as good as toluen) is to pull freebase from the alkaline soup and you can use MEK to clean x-tals in a final step if you want to separate them from other alkaloids.

I salt with HCl and there is no problem with fume as you need only a really small quantity. Plus, if there is too much HCl after salting, it will evap leaving non contaminated mescaline at the end.

Have fun with extraction !
 
Kash said:
If precipitating hcl crystals out of solution you require very fine filter paper most likely, as they pass right through Whatman grade #1 filter papers. #1 filter paper and coffee filters are fine for filtering scraped up hcl crystals from an evaporated salting, though SWIM usually just decants away the liquid. Hope this helps.
Click to expand...

I've found a few things while working with tryptamine that work equally well with mescaline HCL. It's first a good idea to dehydrate the solvent completely. Then once gas is passed through the solvent, distilling off the solvent to leave the salt and recrystallizing from alcohol works great. Or if distilling off the solvent becomes an issue, add water (if solvent is immiscible) and evaporate the water layer.
 
What do you think about these ideas on "dry" extraction:

- use dry cactus powder when possible, having just two phases (liquid, solid) to avoid emulsions completely
- use acids and bases that evaporate (HCl, ammonium hydroxide), so none is left in the plant material
- liquid separation is avoided, filtering is performed instead


The extraction would go like this:

01 ) blend the fresh cacti with a bit of acid to ensure alkaloids are in their salt form
02 ) dry (or better: freeze-dry) the cacti to remove all the water and possibly the acid as well
03 ) grind the dried cactus into fine powder
04 ) de-fat the cactus powder with NPS, stir, decant, filter, completely evaporate the solvent from the powder
05 ) basify the cactus powder using ammonia solution, stir, decant, filter, completely evaporate the ammonia solution
06 ) pull with NPS, stir, decant, filter (keep the solvent this time)
07 ) clean NPS with AC, filter with Celite - this may remove tiny particles then went through filter as well as discoloration
08 ) determine alkaloid content by titration (?) or guess based on dry weight and cactus species
09 ) salt out alklaloids with aqueous HCl solution (DI water used) - same as in Kash's Tek
10 ) evaporate the water, scrape crude alkaloid mix
11 ) cold MEK wash - same as in Kash's Tek
12 ) purify with cold acetone wash OR run a chromatographic column
13 ) salt out purified mescaline OR evaporate the solvent (preferrably in a rotary evaporator)


Ideas are taken from this document on general alkaloid extraction.
 
Some thoughts - I missed this when it first appeared.
05 ) basify the cactus powder using ammonia solution, stir, decant, filter, completely evaporate the ammonia solution
Click to expand...
Mescaline freebase readily forms a carbonate in contact with the atmosphere. Does M carbonate decompose when treated with NPS?

06 ) pull with NPS, stir, decant, filter (keep the solvent this time)
Click to expand...
Which part do you propose to extract with the NPS? The strained cactus solids or the residue from the evaporated ammonia solution?


12 ) purify with cold acetone wash OR run a chromatographic column
Click to expand...
The Nexus would certainly benefit from a bit more practical focus on preparative chromatography. Dry flash springs to mind - pretty simple and forgiving, and performed in a fritted filter funnel rather than an actual column.
 
Does anyone here feel like there is a limit to how many pulls you can reuse the same xye for?

Didnt feel like this question was important enough for its own thread.
 
Same here.
My bottle of cactus xylene has done 20 pulls, give or take a few, and its not gummed up, cloudy, or giving less pure mescaline.
It might help that I defat my teas with paraffin before basing. Paraffin picks up enough stuff that it only lasts two defats before I run the risk of it getting hard to remove after hardening. So sacrificing paraffin might be extending the life of my xylene.
 
So I tried to do the A/B method, boiled 160g of cactus powder, the soup did become more watery as mentioned in the Tek but it was still quite gooey, filtering through a shirt was a pain... A lot of the mud came through, tried to filter with a cotton plug, that was even more difficult... In the end I just basified the liquid, it turned dark, almost reddish black similar to the mhrb soup. And then I was like fuck it let's just add the mud in there as well. I did that, the solution turned reddish brown again, I thought the pH would've come down so I added more base but the color did not change, so added more base... The pH paper now shows pH 14. I then added around 100ml of toluene, gave it a few shakes, kept the soup warm. Emulsions formed but after a while it separated again. I extracted the toluene layer, added benzoic acid (didn't measure, but it was a decent amount, at least a gram or so). Now it's been 3 days and still nothing has crashed out. With the dry tek I did the same, extracted with toluene and threw in some benzoic acid and crystals started to form after 6 hours or so.

So now I'm kinda worried... Have I done something wrong? Should I try sticking the tonight
Toluene in the fridge? Assuming that there is mescaline benzoate still dissolved in the toluene somehow, what would happen if I added dilute HCl to it?
 
Dasein said:
So I tried to do the A/B method, boiled 160g of cactus powder, the soup did become more watery as mentioned in the Tek but it was still quite gooey, filtering through a shirt was a pain... A lot of the mud came through, tried to filter with a cotton plug, that was even more difficult... In the end I just basified the liquid, it turned dark, almost reddish black similar to the mhrb soup. And then I was like fuck it let's just add the mud in there as well. I did that, the solution turned reddish brown again, I thought the pH would've come down so I added more base but the color did not change, so added more base... The pH paper now shows pH 14. I then added around 100ml of toluene, gave it a few shakes, kept the soup warm. Emulsions formed but after a while it separated again. I extracted the toluene layer, added benzoic acid (didn't measure, but it was a decent amount, at least a gram or so). Now it's been 3 days and still nothing has crashed out. With the dry tek I did the same, extracted with toluene and threw in some benzoic acid and crystals started to form after 6 hours or so.

So now I'm kinda worried... Have I done something wrong? Should I try sticking the tonight
Toluene in the fridge? Assuming that there is mescaline benzoate still dissolved in the toluene somehow, what would happen if I added dilute HCl to it?
Click to expand...

Did it cloud? 1g may not be enough to salt all the mescaline. I would add a couple more grams of toluene and throw that in the freezer.
 
Are you sure that mescaline is in the toluene?
Lot of shaking and many pulls are needed to extract mescaline freebase from basic watery soup, it does not migrates to nonpolar very easily.
 
So I put it in the freezer and some stuff crashed out but I think it was just benzoic acid because it redissolve when the solvent warmed up. Also, it didn't cloud at all when I added benzoic acid. So there was no mescaline in there, but then where did it go? 3, 2 hour simmers should've at least gotten something out... I tried the same sample with dry tek and extracted with toluene and ended with some crystals (I didn't weigh them since I had to do a clean up, but they're still sitting on my desk dissolved in water). May be I should shake more and for multiple times? But still... The fact that it didn't pull even a single milligram is... Concerning!
 
Your mescaline is most likely still in the basic water. In my experience, migration of freebase from water to toluene is most critical step in typical A/B two layers liquid extraction.
Wet paste methods are much better - btw. solvent smell could be simply limited by some cover (made from plastic bag) with a hole for the spoon or fork used for mixing.
 
So I mixed the toluene from the previous pull with dilute HCl, then I put it back into the extraction bottle, heated it up in water bath, shook it vigorously and for long periods of time and I did that for several times over more than an hour. Then I pulled it out and added some benzoic acid, no clouding!

I mixed it with HCl again, will do another pull or two and after that I'll evap the HCl solution. It is cloudy but seems like it's mostly fat and/or other stuff. Is there any other possible way of saving this extraction? May be neutralize the whole soup, evap all the water and try the dry tek? That'll be a lot of work...
 
Listen to others advice I'm just trying to see if I understand enough of the process on my own.

You likely pulled all the alkaloids with the HCl aqueous layer and the toluene should be void. Adding benzoic acid shouldn't do anything to the already acidic layer... and if you added to the toluene it is likely void of alkaloids so nothing precipitated.

If you were to evaporate the HCl solution you should have all your alkaloids which if too 'dirty' you could make it basic again with NaOH until around 12-13 then add toluene to pull the free alkaloids again. Then add the benzonic acid aqueous layer to the toluene which should cause it to percipient?
 
No I think you misunderstood me, I pulled with toluene, added benzoic acid to the toluene but nothing crashed out, so I mixed that toluene with HCl, made another pull, added benzoic acid again, and again no clouding. I only mixed with HCl after nothing clouded with benzoic acid.
 
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