2nd Mescaline Extraction - How to Purify?

[blue.magic]

After successfuly trying Kash's A/B Tek on 2 smaller T. Pachanoi samples, I tried to extract usable amount of mescaline from about 1 kg (raw outer flesh - should be an equivalent of 100g powder I guess) of T. Peruvianus. Unfortunately, I ended up with just a green-reddish oily gunge and I don't know how to properly purify this:

Some more extract has been recovered from the Pyrex dish by washing it with small amount of water and dried on an hourglass:

The product has been tested by Marquis and Mecke reagents. It seems mescaline is present:

How to purify this?

I know about three options:

1) Cold MEK wash. This should however be used on crystals so I am not sure it would work on this.

2) Phlux's Quick Mescaline HCl Recrystallization Tek.

3) Repeat the process: Dissolve in water, basify, precipitate freebase, dry, redissolve in toluene, salt out with dillute HCl, pull, recrystallize in water. But this seems like many steps which may lead to a huge loss of product.

My final goal is to obtain a reasonably pure mescaline HCl or fumarate.

Some notes on the extraction:
The cacti were peeled and cut, refreezed three times, blended, cooked and filtered seven times w. citric acid, reduced, filtered, de-fatted (3x w. toluene), basified w. lye, pulled (4x w. toluene), salted w. about 0.6 ml HCl in 100 ml water. The toluene pulls were already light green colored.

 

[endlessness]

I'd re-a/b it, it's the best way I've found to really clean up oily goo/dark mesc.. I must say I didn't try phlux's re-x method though.. You could try two different methods and compare, and let us know, if you want

 

[blue.magic]

I'd re-a/b it, it's the best way I've found to really clean up oily goo/dark mesc.. I must say I didn't try phlux's re-x method though.. You could try two different methods and compare, and let us know, if you want

Okay I've re-A/Bed it (what a word :lol: ). The toluene layer seems to have captured some impurities but the water layer is still greenish:

Anyway. Pulled the water layer and letting it to dry.

I also tried the Phlux's method: took 100 mg of the gunk-extract, dissolved in 5 ml of water, added 100 ml of acetone and stirred. Some white flakes precipirated appeared almost instantly and slowly descended to the bottom of the beaker:

It's hard to see the precipitate from the photo. This mescaline HCl looks much nicer but it's also very little amount.

I will let it the precipitate in a fridge overnight and continue later...

Even at 0.1% yield, the expected amount of mescaline from 2 kilos of T. Peruvianus was about 2 grams - this seems to have 100 mg at best. Either the cacti were really weak (much weaker than good old San Pedros) or something went bad during the extraction process ¯\_(ツ)_/¯

 

[antichode]

If it's HCL just dissolve it in acetone. This will leave you with a fairly pure tan powder.

Endlessness is correct that a re AB will make it super clean but you'll lose some goods along the way.

I think you will be satisfied with the acetone wash

 

[antichode]

For future extractions I would highly recommend sulfuric acid to salt. If you add this drop wise to your water layer with a lot of stirring untill PH 7 is reached and stable. You will recover very pure mescaline which will crystallise directly from the water when reduced and cooled

 

[antichode]

Also for what it's worth. I think you've over complicated things (as most do). Try adding base directly to fresh blended cacti untill its watery. add solvent and blend on high for a few minutes. Keep it hot at 80deg c. Pull solvent three times and salt once as above.

All this freezing and boiling and filtering is a giant waste of time imo

 

[blue.magic]

For future extractions I would highly recommend sulfuric acid to salt.

Concentrated or dillute? Not sure about the H2SO4, but even a single drop of HCl can already be too much... In the end, one has like 800 ml of toluene to which about 100 ml of acidic water is added. It is very hard to measure pH from the bottom water layer. The pH paper gets coated in toluene and thus often does not measure true pH of the bottom water layer. Even when stirring vigourously, the water droplets won't make it to the surface to be measured. I still have not figured out how to properly do this acid salting step.

Also for what it's worth. I think you've over complicated things (as most do).

Well - like most people - I am not a chemist or skilled extractor so I have to stick with popular and well-tested Teks available in the wiki. Better waste few hours of time than kilos of precious cacti.

I have not found the technique you describe on the web. If you have any references to it, please provide. It looks like some kind of STB tek but the only STB tek for mescaline has been removed from Wiki.

If you have such simple and efficient Tek, then maybe try to promote it to wiki so people won't use the complicated ones...

Also I would rather use complicated technique with high yield and purity in the end.

Thanks for the acetone wash advice. Will try it next time.

 

[endlessness]

If it's HCL just dissolve it in acetone.

Do you mean wash it in acetone? Because mesc HCl should be practically insoluble in acetone. Or maybe you meant to say dissolve the impurities in acetone.

And while I love acetone washing, when the mescaline is black or very very impure/dark/goeey, the wash itself doesn't seem to clean too much ime.. When it's cleaner, like tan, then yes the wash works well..

Unless you have some specific tip to work in such situations? Or has it worked for you even when it's very impure?

 

[blue.magic]

Okay here are the results. Both re-A/B and Phlux method resulted in another goop - now brownish-black. It tastes very bitter.

At least this time it's more homogeneous. The Phlux method seem to purify the mescaline.HCl better, but since it is very hard to decant acetone-water without losing the floaters, they recombine with impurities. The result is at least more solid than liquid.

Both methods caused substantial loss of amount (over 60% I guess).

I'm giving up. Some lessons learned:

- try distilled/DI water next time (maybe minerals affect the salting?)
- try less acid for cooking next time (the citric concentrated too much when reducing the water amount - over 100 grams in 400 ml of cactus tea)
- try less HCl for salting next time (seems resulting in 'black' mescaline)
- experiment with smaller batches and other extraction routes (dry and powderize cactus first, then defat while dry instead defatting the tea)

 

[downwardsfromzero]

The pH paper gets coated in toluene

You know, you could use a pipette to take a drop of the aqueous layer and measure the pH by dripping it onto the paper? Or even just wet the paper with distilled water first.

 

[blue.magic]

You know, you could use a pipette to take a drop of the aqueous layer

Stupid me... of course.

I need to learn molarity calculations and how various acids affect pH. I too often add just a drop and pH falls too much or vice versa (with strong bases). Or I dillute it too much and then end up with lots of extra water ... just unable to find the right balance.

It seems to be essential for the mescaline extraction as one needs to add just the right amount of acid. I am not sure if this proper amount can even be resolved with a pH paper (the colors around pH 7 are almost the same).

Maybe drain the water from sep. funnel, measure pH with a pH meter, add carefully calculate amount of acid, put the water back in funnel, shake, repeat.

 

[downwardsfromzero]

I am not sure if this proper amount can even be resolved with a pH paper (the colors around pH 7 are almost the same).

Look into obtaining a set of narrow-range pH papers, or a pH meter.

 

[blue.magic]

I am not sure if this proper amount can even be resolved with a pH paper (the colors around pH 7 are almost the same).

Look into obtaining a set of narrow-range pH papers, or a pH meter.

Thanks. I have both the narrow range papers (for measuring urine pH) and a pH meter - I don't use the pH meter much as it needs to be calibrated and it takes over minute to get a readout. The mistake was adding too much acid and I really don't know how much to add, how to dillute it etc.

Some people on the forum say one has to guess the amount of alkaloids, then compute the molar weight of acid to be added etc.

To makes things even more complicated, I found some acids and polyprotic meaning the pH can jump suddenly two or three times during acidification. Fortunately, this is not the case for HCl as it is monoprotic.

I know I am overcomplicating things probably, but I really like the technical/controlled approach so the results can be solid and predictable.

 

[antichode]

Hey dude

It's nice and simple. Get this product API® Products

It comes in a dropper bottle and is about 80% sulfuric. You just add one drop at a time to our water. Shake it vigorously with your solvent. Pull off a sample with a pipette and pour over your ph meter tip (I do not recommend papers but it works for some). Your looking to reach ph 7. Hopefully your water is showing to be quite basic once mixed. A high ph while continually adding acid is a good sign as it means lots of mescaline freebase is in solution. You'll get a feel for it over time just be careful how much oh add as it approaches 7. It can fall off a cliff really fast and end up at a low ph all of a sudden. If you go drop by drop you'll be fine though.

Something I've noticed that is a visual indicator. Very little emulsion is formed when the ph is above 7. When it drops below 7 emulsions start to form and are very hard to clear.

Good luck

 

[downwardsfromzero]

Re: narrow range papers - I was fortunate enough to obtain a set with six different pH ranges: 1-4, 4-6, 6-8, 8-10, 10-12 and 12-14. Admittedly, the resolution around pH 7 is still only half a unit but the set is nonetheless quite useful. I still hope eventually to get a pH meter, of course.

 

[blue.magic]

Pull off a sample with a pipette and pour over your ph meter tip (I do not recommend papers but it works for some).

Thanks. I thought the pH meter should be immersed in a liquid to work. If just pouring a sample on the glass electrode would work, then great

In my case, a single drop of acid was already too much. But this was 0.5 mL or 35% HCl.

Another idea I had was to sample the alkaloid-laden solvent, add water containing a pH indicator, then add tiny amounts of acid until the water layer changes color from basic to neutral. This way one can determine the amount of acid required. Maye some even some natural pH indicators could be used (e.g. beetroot).

BTW I did a cold anh. acetone wash, filtered and kept the "solids". The purified stuff was still reddish-brown goo with some tiny mescaline.HCl crystals in it. The total weight is unfortunately <50 mg. I still don't know what went wrong - expected at least several grams when starting with over 2 kilos of T. Peruvianus. Maybe the de-fatting with toluene (bad solvent for that step?), maybe not using distilled water for acid-salting, maybe using way too much acid or base in the A/B extraction (I certainly overshoot the basing).

 

[antichode]

2g from 2kg fresh sounds within the ball park but I wouldn't expect more. I only have three out of over sixty plants that produce yields over 1% most are about .5%

The best thing I ever brought was my PH meter and a 50ml glass pipette with a nice fine tip and rubber bulb like this http://www.camlab.co.uk/images/thumbs/0008923.gif
This give you enough volume to pour a steady stream over the electrode and get a stable reading. I think once you master the titration you'll be much happier. And stop messing about with boiling filtering, freezing and defatting etc. Avoiding emulsions is simple..

Heaps of base (I use 20% the wet weight of cactus)
Enough solvent ( I use 20% of the final volume)
Heat and time (80 deg C will separate anything quite fast)

 

[endlessness]

Antichode, did you ever try a dry tek to compare yields? I've always gone A/B with cact as you mentioned, but am curious on how freebase mescaline's slight water solubility diminishes yields in A/B, versus dryteks. At least anecdotal reports (and my own experience) seem to suggest that unlike DMT, with mescaline you can keep doing multiple pulls beyond the 3rd pull that still yield significant amounts.


By the way, regarding salting difficulties, I agree a pH meter and being careful with titration works wonders.. Alternatively there is a simple method that doesn't need careful measurements which is doing FASA/FASI and getting mescaline fumarate. I've found it works very well and is a beautiful process to behold

 

[antichode]

Antichode, did you ever try a dry tek to compare yields?

Hey Man

Yeah I cut my teeth on Rons tek (and all of he others on the nexus) and it seemed to work wel,l comparable I would say. But with one caveat. You have to get the initial basing water ratio right. Too little and I think you lose solvent to the dry cactus. Plus drying cacti then grinding it takes so long!

These days I skip the initial acid cook and just go STB I've found my yields shot up once I started doing this. I think the reaction that breaks down the cactus is superior in releasing mescaline in all respects (boiling,freezing,dry the grind etc). plus it heats itself up in the process saving you time again. And the final reason for my STB preference is that it's scalable. Dry teks really aren't useful once you get above a certain weight

 

[blue.magic]

The best thing I ever brought was my PH meter and a 50ml glass pipette with a nice fine tip and rubber bulb like this http://www.camlab.co.uk/images/thumbs/0008923.gif

Have this exact one and some long 50 ml pipettes as well. So will try! I like the "release valve" so one can run the liquid slowly. Probably no need for a burette.

I think once you master the titration you'll be much happier. And stop messing about with boiling filtering, freezing and defatting etc. Avoiding emulsions is simple..

You mean by controlling pH not getting too low or too high will avoid emulsions? If this is the main/sole reason for having emulsions, than that's great!

Heaps of base (I use 20% the wet weight of cactus)
Enough solvent ( I use 20% of the final volume)
Heat and time (80 deg C will separate anything quite fast)

Very helpful, thanks.

I am a bit worried about adding so much base (e.g. for 1 kg wet weight, that is 200 g NaOH - which is a LOT). That much base will run the pH very high, which may in turn break some good alkaloids (hordenine, mescaline) and saponify the fats.

Anyway, I am thinking about using a 2 L beaker with hotplate stirrer (it is the upper limit my hotplate can handle), then adjusting heating to settle on 80 deg C and letting the basic soup mix for few hours. Then continue by pulling.

I would still do at least the acid soak since the natural salts may hold the mescaline, don't you think? I've read somewhere that some salts (e.g. tannates) bond so strongly even strong bases like KOH may not liberate the alkaloid. So converting to different salt like citrate or acetate first may be helpful. This may however be more related to MHRB/DMT rather than cacti.

Alternatively there is a simple method that doesn't need careful measurements which is doing FASA/FASI and getting mescaline fumarate. I've found it works very well and is a beautiful process to behold Smile

Good to hear this may work for initial extraction. I did this for purification stage and it worked miracuously.