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Acid/Base/Acid Mescaline Extraction


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#1 Phineas_Carmichael

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Posted 11 August 2011 - 11:26 PM

It has been speculated that combining the techniques of an A/B DMT extraction with Waylitjim's Mesc Extract Tek and Irishlions Cactus Tea TEK might be a good way to go about getting nice pure mescaline with household chemicals.

My buddy Freddy has been dicking around with this idea. The basic procedure goes like this:

1.) 100g powdered San Pedro cactus is bundled in an old dish towel. This forms a sort of "tea bag" which will be used in the next step.

2.) The "tea bag" is steeped in boiling water slightly acidified with HCl. 5 pulls (3 acid, 2 d-h2o), about 45 minutes each, with gentle squeezing after each soak. Too much squeezing will force the cactus powder through the towel, we just want the water.

3.) Approximately 2.5L of acidic San Pedro Tea is reduced to ~500mL.

4.) The reduced solution is defatted 5 times (3x toluene, 1x toluene/xylene, 1x xylene)

5.) The defatted solution is basified. A solution crafted from 450mL d-h2o and 150g NaOH is used.

6.) The basified solution is extracted with 100mL xylene

7.) The xylene (containing mescaline freebase) is salted with 100mL of a sulphuric acid solution. This solution is created by adding 10 drops of "battery electrolyte" to 350mL d-H2O.

8.) Steps 6 & 7 are repeated using the same 100mL xylene and fresh sulphuric acid solution each time.

9.) The resulting 300mL water is evaporated to yield crystalline mescaline sulphate.


No pictures of the process, but here's a couple pics of the product:
DSCN3713.JPG

Comments? Criticism? Scathing indictments?

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  • DSCN3709.JPG

Edited by Phineas_Carmichael, 11 August 2011 - 11:38 PM.
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#2 gonefishen

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Posted 11 August 2011 - 11:36 PM

swim doesnt really understand how you did it but thats awesome bro.
swim is ordering some torch and plans to try a similar process.. do you think u could do it with fresh cacti?

#3 TurkeyRanch

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Posted 11 August 2011 - 11:52 PM

I have been making a lot of tea lately, and thinking along the same lines. . . Awesome as always Phineas.:bow:

What was the yield? Any plans on an acetone wash to clean it up?
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#4 Phineas_Carmichael

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Posted 12 August 2011 - 12:03 AM

swim doesnt really understand how you did it but thats awesome bro.

1.) Make Cactus Tea-Bag.
2.) Boil tea-bag in slightly acidic water until cactus is no longer bitter.
3.) Boil cactus-water down to less than 500mL.
4.) Add 100mL toluene (or xylene or both) and separate. Repeat 5x. Discard non-polar and retain cactus-water.
5.) Create a solution using 450mL H2O and 150g NaOH. Add this to the cactus-water.
6.) To your now ~900mL basic cactus-water add 100mL xylene. Separate and retain the xylene.
7.) Add 100mL sulphuric acid solution (created with 350mL H2O and 10 drops "battery electrolyte") to the previously mentioned xylene. Separate the solutions.
8.) Evaporate the sulphuric acid solution.
9.) Repeat steps 6, 7, & 8 using the same 100mL xylene and fresh 100mL acid each time.

Here's what's happening chemically:

1.) First we encourage the mescaline in the cactus to be mescaline in our water. We do this with an acid, which forces our mescaline to be a salt. Which salt depends on which acid we use; hydrochloric acid will form the hydrochloride salt, citric acid the citrate salt, etc. Not important anyway, just so long as we force all the mescaline in the cactus to be a salt in the water.

2.) Then we take that acidic mescaline-containing solution and reduce it on the stove-top to a volume that is easy to work with.

3.) Defatting. Mescaline salts are very soluble in water and not very soluble in non-polar solvents like xylene and toluene. Cactus fats and tannins are very soluble in non-polar solvents and not very soluble in water. By mixing and separating xylene or toluene into our acidic cactus-water we are removing the fats and tannins while allowing the mescaline to stay in the water.

4.) Basification. By adding an excess of NaOH we force the mescaline salts back into their freebase form which doesn't like to be in water.

5.) Extraction. Mescaline freebase is highly soluble in xylene, but not hardly at all soluble in water. By adding a bit of xylene to our basic cactus-water we force the mescaline into the xylene.

6.) Salting. Mescaline freebase is a caustic oil, decidedly difficult and dangerous to work with. We want a shelf-stable solid mescaline salt so we can put it in a bottle and look at it. Remember that mescaline salts are highly water soluble and not at all soluble in xylene. By exposing our mescaline freebase-containing xylene to weak sulphuric acid solution we force the mescaline back into the water.

7.) Evaporation. Evaporating that water gives us impure crystals of mescaline sulphate. Again, which acid you use will change the end product; sulphuric acid will give the sulphate, hydrochloric acid the hydrochloride, etc.

swim is ordering some torch and plans to try a similar process.. do you think u could do it with fresh cacti?

Absolutely. Just follow Irishlion's tea Tek, defat and basify the solution, then pick up with Waylitjim's extraction.

What was the yield? Any plans on an acetone wash to clean it up?

1.361g sulphate salt (*EDIT* by stoichiometry, this is equivalent to 1.171g of the hydrochloride salt)

No plans for an acetone wash yet. Freddy and I are unsure that mescaline sulphate can be purified in the same fashion as mescaline hydrochloride.

Edited by Phineas_Carmichael, 01 September 2011 - 07:24 PM.
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#5 Windy

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Posted 12 August 2011 - 01:08 AM

Household chemicals?

#6 SGT.Goomz

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Posted 12 August 2011 - 01:13 AM

:eusa_clap

#7 Phineas_Carmichael

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Posted 12 August 2011 - 01:23 AM

Household chemicals?

Yes.

1.) Muriatic acid concrete cleaner. Available at any hardware store worth its salt.

2.) Sodium hydroxide drain cleaner. Available (with a little searching) at small (not big-box) hardware stores or online at soap-maker's websites.

3.) Sulphuric Acid. Available as "Electrolyte Solution" or "Battery Acid" at auto parts stores.

4.) Xylene. Available as a paint thinner/stripper at hardware and paint stores.


I'd classify all these things as "Household Chemicals," but then again I come from a strange house; at my house we have dirty concrete, clogged drains, a motorcycle with a broken battery, and walls that need to be stripped before we re-paint them... ;)
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#8 Windy

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Posted 12 August 2011 - 01:31 AM

:lol:

#9 Defiance

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Posted 12 August 2011 - 02:10 AM

Very nice work Phin!

If you evap the HCl salt out and then clean like Tregar with acetone before re-basing and forming the sulfate salt you can build some pretty awesome crystals. Just looking at your pic, even the brownish product really looks like it wants to form some nice crystalline structures.

It's pretty important to monitor pH when forming sulfate salts since it won't evap off like HCl will. You'll need a bigger dose with sulfate because of the increased molecular weight and all that.

The only nit I'd pick is that you don't have pure mesc with no cleanup step, it's still a broad spectrum extract of every alkaloid in the botanical.

I'd love to get TLC spots after an acetone cleanup just to see if it really does get rid of everything but mesc.

#10 Ferretious

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Posted 12 August 2011 - 02:34 AM

Muriatic acid is the only avaliable acid where I'm from. I'm sure it will work in the last step just as well if not better than sulphuric.
Well done Phin'!:headbang:
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#11 SilvrHairDevil

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Posted 12 August 2011 - 10:36 AM

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#12 gonefishen

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Posted 12 August 2011 - 11:32 AM

"1.) Muriatic acid concrete cleaner. Available at any hardware store worth its salt.

2.) Sodium hydroxide drain cleaner. Available (with a little searching) at small (not big-box) hardware stores or online at soap-maker's websites.

3.) Sulphuric Acid. Available as "Electrolyte Solution" or "Battery Acid" at auto parts stores.

4.) Xylene. Available as a paint thinner/stripper at hardware and paint stores."

thank you phin thats the info swim needed.

#13 Phineas_Carmichael

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Posted 12 August 2011 - 01:39 PM

Id love to get TLC spots after an acetone cleanup just to see if it really does get rid of everything but mesc.

You know, so would I...

TLC plates were created as follows:

10g Corn Starch
3.5g Plaster of Paris (Calcium Sulfate Hemihydrate)
15-20mL D-H2O

The mixture was applied to microscope slides, approximately 2mL per slide.
DSCN3721.JPG

Chromatography will be carried out when the plates are completely dry.

#14 Defiance

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Posted 12 August 2011 - 02:24 PM

Oh shit, it's on.

#15 Phineas_Carmichael

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Posted 12 August 2011 - 08:08 PM

Oh shit, it's on.

Yes, it is most definitely on. :nunchuck:

First, an acetone mortar & pestling is in order.

~1.1g brown mescaline HCl from a previous extraction:
DSCN3726.JPG

A splash of anhydrous acetone is added and the mixture pestled for about 2 minutes:
DSCN3727.JPG

Then filtered and dried:
DSCN3729.JPG

And scraped and quantified:
DSCN3732.JPG

A small amount of crude product was saved and it's chromatography time! :dance:

According to Freddy, there was some difficulty in choosing solvents. What a pain in the ass! Water doesn't dissolve the impurities, acetone doesn't dissolve the mescaline, xylene stinks too much, etc etc... Finally a mixture of 5:4:1 hexane:acetone:water was used to dissolve the samples. It was perhaps not the best choice, but the best that could be done.

The plates were spotted (sloppily) with the mescaline containing mixture and run through TLC using 6:4 hexane:acetone as the mobile phase.

Both plates after developing; unwashed sample on the left, washed on the right:
DSCN3762.JPG

Unwashed sample under black light:
DSCN3766.JPG

Washed sample under black light:
DSCN3769.JPG

This bears repeating with better technique... :eusa_thin

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  • DSCN3730.JPG


#16 Defiance

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Posted 13 August 2011 - 08:36 AM

I'd keep at it, actually. It can take more than one time through a development bath to get good separation (Here's a great example) . You can see that at least one constituent is mobile really well under black the black light.

I've never run TLC on mesc before so I don't really have any input on your solvent system. It looks pretty good, stuff is moving. It may run right off of the plate though, and then you have to swear and tweak your solvent some.

You didn't mention it (or I missed it) in your posts, but did you activate the plates? A half hour in a 250F oven will drive off the excess water and help with mobility. Plaster of paris will form the dihydrate when you mix it with water and take its' sweet time to come back around to the hemi-hydrate but between 200F - 300F the process is accelerated.

I really think you're right where you should be for homemade plates.

Edited by Defiance, 13 August 2011 - 08:47 AM.


#17 Phineas_Carmichael

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Posted 13 August 2011 - 01:12 PM

I really think you're right where you should be for homemade plates.

Thanks for the kind words buddy. This has been an interesting experiment for Freddy, it's been fun to dick around...

Yep, plates were activated at 200F for half an hour in the original tests. In today's trial, plates were activated at 250F for 45 minutes, samples were dissolved in acetone/isopropanol, and a few drops of glacial acetic acid was added to the mobile phase.

Both plates after developing once:
DSCN3772.JPG

Unwashed sample under UV:
DSCN3781.JPG

Washed sample under UV:
DSCN3785.JPG

Unwashed sample left, Washed right, twice thru the developer:
DSCN3788.JPG
The top band is much "redder" in the unwashed sample, doesn't show too well in the photograph... :eusa_thin

Edited by Phineas_Carmichael, 13 August 2011 - 01:51 PM.


#18 Phineas_Carmichael

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Posted 19 August 2011 - 01:22 PM

Freddy tells me he's still tweaking his chromatography system, with little progress. Longer plates might be the solution...

In any case, he wrapped up this cactus acid/base/acid and came out with ~2.6g impure sulfate salts:
DSCN3801.JPG

Stoichiometrically this is equivalent to ~2.3g HCl, so either Freddy has high-alkaloid San Pedro or some kind of experimental error.

Mortar & pestled 2 minutes under freezer cold acetone to yield this (2.4g):
DSCN3804.JPG

:dance:

Edited by Phineas_Carmichael, 19 August 2011 - 04:14 PM.

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#19 Defiance

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Posted 28 August 2011 - 12:38 AM

Hmm. I might give silica gel a shot as a substrate too. I've heard that it's tough to grind. I've only used prepared TLC plates, but they're expensive.

That 2.4g looks really, really nice.

I'd bet the difficulty getting a good separation comes from the similarity in alkaloids present?

Edited by Defiance, 28 August 2011 - 01:50 AM.


#20 Phineas_Carmichael

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Posted 28 August 2011 - 09:38 AM

I'd bet the difficulty getting a good separation comes from the similarity in alkaloids present?

That and a total lack of fluorescamine and/or ninhydrin on Freddy's sloop. A book called The Analysis of Controlled Substances gives a TLC system for mescaline but there's really no home-chromatography equivalent of the fluorescent developers...




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