I've been following a procedure that is based on Kash's A/B procedure. 100g cactus powder is placed in cheesecloth and covered with 800ml water and 200ml vinegar, and pressure cooked at 15 psi for 20 minutes. The liquid is poured off and this procedure is repeated for a total of five times. The liquids are combined and boiled until volume is reduced to 900-1000ml, and then basified with 200g KOH (pH >14). This solution is then extracted with 5 portions of 150ml xylene. The organic layers are then combined and mescaline HCl is formed by addition of 20-25ml dilute HCl (prepared by adding 8-10 drops of 35% HCl to 120ml distilled water). The aqueous layer is filtered off and set aside, and then the addition of 20-25ml of dilute HCl and filtering off is repeated for a total of 5 times (until the prepared dilute HCl solution is entirely consumed.) The aqueous layers are combined and allowed to evaporate.

My yields are typically 0.1% to 0.2%, the former using san pedro powder and the latter using a bridgesii powder. I'm not sure if it's because my powder is weak or my procedure/technique is lacking. Any suggestions on how I can improve technique? When mixing with xylene, I typically roll and shake the bottle for a few minutes, allow the layers to resolve, roll/shake again, and so on for a total of 4-5 times for each of the 5 extractions. I follow the same procedure with the addition of dilute HCl.

I've also heard of people adding HCl to the organic (xylene) layer serially, rather than combining the layers and adding HCl, as I do. Would this improve yields any?

Have you tasted the waste? Is it bitter? Yes - you are losing mescaline. No - you can bin it.


I would HCl titrate here every xylene pull separately. Then you will exactly know how much mescaline is in each pull, so you can decide when to stop and you are sure there is not much left behind in th water.


Above steps can make you more certain what you left behind and what you continue with.

Of course you can try different approach and compare results

I do see a few issues.
I dont envy you working with powder People say the extraction is more complete that way but I think avoiding all the mess by extracting chips is well worth the extra boiling. But thats an old debate and up to the individual. Boiling cactus powder in a pressure cooker can be dangerous, though. Not so dramatic with modern pressure cookers but still, something could clog. Anyway, the cactus chips or powder should initially taste quite bitter. After the goodies are boiled out the squeezed solids should not taste bitter, this is actually a good gauge to tell when you've done enough boils. Just keep boiling and squeezing until the solids dont taste bitter. You probably werent far off, 3 boils might have done it, 4 probably would have, 5 almost certainly should have if you were actually filtering/squeezing most of the liquid out after every boil.
You probably used significantly more KOH than really needed, I most likely would have used a quarter of that amount. Using more than needed would not reduce yield, though, if anything it would increase yield by a small amount. I work at the low end so the cactus lye sludge goo isnt quite as dramatically dangerous to human flesh. Again, thats an old debate.
I notice one big thing, no pH check. You used enough HCl to make roughly 3 grams of mescaline while obtaining 0.1-0.2 grams of product. A great excess of HCl will give you a lower quality product and you have to deal with the corrosive fumes while evaporating. There is no need for successive acid washes to salt the mescaline the way that successive xylene washes are needed to extract the mescaline because mescaline hydrochloride is not soluble in xylene. You should really, really get some pH papers so you can see when the aqueous layer gets to neutral or slightly acid and stays there. The closer to a stable pH of 7 you can hit, the cleaner your product and the less HCl fumes when you dry it. 1-14 pH papers can be got very cheaply on auction sites and you can also get them in pool supply shops and most pet stores for somewhat more money. The ultra cheap packs from china sold on auction sites work just fine. You could even stain absorbent paper with juice from raw purple cabbage and use that as pH paper if you really had to [do a google image search for purple cabbage pH].
As for your technique, if your discarded boiled cactus solids were no longer bitter then I'm guessing you got out and obtained nearly all of the mescaline. Your work with the xylene sounds like it should be sufficient. I enjoy the luxury of separatory funnels and my home made magnetic stir plate but I could do it like you do and still get all the goodies. Your source material is likely the biggest issue, 0.2% isnt unheard of for bridgesii even though they can exceed 1.2% and 0.1% is about normal if your pachanoi is the 'PC', aka. 'Backberg' clone.
I'd really encourage you to track the pH when salting. But most of all never throw out boiled cactus without tasting it first.

[quote=pete666] Have you tasted the waste? Is it bitter? Yes - you are losing mescaline. No - you can bin it.

Is this a effective way of testing alkaloid strength of a mescaline containing cacti or just a way of seeing if all the cacti snot has drained into the tea?

Mescaline is bitter. If you are after mescaline, you will hardly find it in something not being bitter

I'll try these suggestions next time around. I did taste the acid boil solution and it did taste slightly bitter, but it never seems to go away even after like 7 boilings.

I'm giving it a second try with a new batch of SP powder. Started with ~250g of powder, pressure cooked eight times with 1800ml water + 200ml vinegar per iteration. Each one tasted bitter but I ran out of vinegar and if eight boilings don't get it all, oh well. Final volume was reduced to about 2000ml, so I'll do the extraction and salting in two batches. This time around I think I will try making the sulfate salt and running a binary solvent recrystallization with acetone and water, since my HCl salt crystals were ugly last time. I'll be sure to watch the pH, as I know that sulfuric acid doesn't evaporate like hydrochloric acid.

Have you seen this ?

I have, but I didn't feel like obtaining MEK. I think that sulfate crystals are generally better looking, too?

MEK is not necessary. Acetone and IPA will do the job.
Even activated charcoal is not necessary if you are OK with slightly off-white mescaline
Charcoal is important if you want to have clear solution when you dissolve the result in water. If you don't purify it with charcoal, it turns from almost white powder to brown solution when dissolved in water, because there are invisible impurities within the molecular lattice.
Sulfate is OK if you don't have the blessing of possibility to use rectal ROA. (Its water solubility is low)

How thorough do you mix your pulls, and for how long? You should do several cycles of mixing/letting stand before separating each pull.

Also, did you try salting your last pull separately, to see if proportionately it has a large amount of mescaline? Because that would give you a good indication if you need to keep pulling. IME mescaline is way more stubborn to move out of the cact and into the non-polar compared to DMT, for example.

endlessness, I think he has a problem not with unability to pull from water to non-polar, but rather with unability to exhaust the cactus and to move the mescaline from tissue to water.
I don't use A/B, so I am not boiling anything (thanks to STB), but eight boils sounds unbearable.
If I had bitter tissue after 3 boils, I would change the TEK

Hmmm yeah I see what you mean I had missed that.. though, with powdered cact AND pressure cook, I find it hard to believe that he isn't exhausting the cact after that many boils.

Also, I understand the logic behind it but did anybody ever cross checked with some analytical method or at least a separate pull to see if bitterness does indeed equate to significant yield being left behind? Is it possible a very tiny amount of maybe even non-mesc alkaloids will make it bitter and yet not be worth to extract?

Same as with non-polar pulls, I suggest doing the last boil separately, that way you can extract from it and see if there is anything significant coming out of it, if it's worth to do yet another boil or not.

Yes, it is good to know as much information about ongoing extraction as is possible.

I do separate titration for every non-polar pull. Immediate feedback this way
Can be done for A/B as well, of course

I wanted to do a STB but I hear even the best procedures can sometimes give emulsions. I'd rather waste my time boiling and straining than risk having to toss everything because the emulsion can't be resolved.

Every emulsion can be resolved.

But I get what you mean. Our TEK still needs some tweaks to make it reliable with complete cactus without emulsions, not just with green tissue. I have some ideas how to improve it, I just need fresh cactus, which is currently growing

Sure, if you have the glassware to add more and more base and water. Maybe next time, when my own cacti are growing, I'll try a STB method. It does look easier.

No, in my experience, adding more base with STB hardly resolves any emulsion for initial extraction. There is usually too much base to have any effect.
In fact the base is the reason of the worst emulsions.



Observe this topic. I will have plenty of fresh cactus and getting just the green tissue is a lot of work, so motivation to find working way for whole fresh cactus is high.

I'll have to read through your posts today/tomorrow. I really appreciate how thorough you are in your procedures!

I'm almost done with the sulfate salting. As I said, 240g of starting material was boiled and reduced to two solutions of ~1000ml each, and each extracted with five portions of 150ml xylene. I acidified the organic layers with dilute (approximately 10% v/v) sulfuric acid, but I ended up undershooting the pH of one solution, so I had to chase it with small amounts of acid and base until I reached a pH of ~6.

The aqueous layer of one of the solutions (the one where I had to chase the pH) is slightly yellow, whereas the other one, which I titrated perfectly the first time, is almost crystal clear. Weird. The yellow one does smell slightly of xylene, but no layers are forming. I wish I had a distillation setup so I could boil off any xylene, but oh well.

I'm hoping for 0.5% yield from dry starting materials... but that's probably wishful thinking. On an (un)related note, I really need to buy myself a sep funnel. Decanting with over the counter instruments is a pain in the ass!

Xylene forms an azeotrope with water [the mixture boils lower than water], a few small traces are very easy to cook off of a solution. I use a coffee maker hotplate, as it heats water to nearly the boiling point of water-xylene without ever reaching the boiling point of water. It works so well I'm not afraid to drink the resulting water, in small single-dose amounts. Thats how I avoid messing with DMT goo or bothering to get DMT fumarate crystals.

I hate undershooting the pH during mescaline saltings, even with HCl since it leads to a less pure product as you noted [that yellow leads to orange mescaline and its a sticky black goo in its pure state] and I dont like having to add base to a solution that should just be mescaline and water. Theres one trick I use to minimize the risk.
Mescaline is somewhat soluble in water, you'll experience this when salting because you'll add a little acid and the water will still be like pH 8.5 due to a portion of mescaline freebase being dissolved in the water. While one can pull all the mescaline into water in one salting, with luck hitting pH 7.0, what I more often do is salt some of the mescaline into one portion of water, test the pH and set it aside, then do the same with another portion of water and add it to the first. These should be pH 7.5-9. Then if you undershoot on the last salting 1) it'll only effect a fraction of your mescaline and a smaller volume of water 2) you can slowly add it to the previous combined portions while monitoring pH, that free mescaline will help neutralize the excess acid 3) if you undershot by very little the final mix will still be basic and you can very carefully add the last needed quantity of acid without xylene being in the way, complicating things.
The pulls taken off when its still basic are quite clean, that yellow gunk comes over a little at neutral and a lot once you reach and go below pH 6. Whatever it is, its a weaker base than mescaline.
Its a good idea to have some very weak acid for the final stage of salting. I use 1M HCl for most of my salting, but I switch to 0.1M HCl at the very end [the equivalents with sulfuric acid would be 0.5M and 0.05M. 10% sulfuric acid is 1.02M, so not bad for most of the salting if your careful but some weak stuff would help at the end.]
The yellow/orange gunk can be removed by recrystallization or anhydrous acetone washes.