Botched Mescaline Purification (pictures)

[blue.magic]

I followed the Kash's A/B Mescaline Extraction Tek to the letter and obtained 389 mg of mescaline.HCl extract.

I decided to purify the extract using further instructions form the tek. I don't know how to better estimate how much toluene, fumaric acid etc. use for my input amount, so I simply scaled all weights and volumes.

The last two steps are confusing to me:

6. Add the fumaric methanol to the toluene and mix it alittle. After a short time, the solution turns cloudy and crystals begin to form. Once crystals settle, mix it alittle more and pour into a dish.

7. Very carefully decant by pouring off liquid and leaving behind white crystals. With no remaining liquid on the plate, let crystals dry and scrape up, yielding pure white Mescaline Fumarate. Enjoy!

I mixed the substances (step 6.) and observed a cloudy solution immediately. However, the toluene separated from the methanol layer and now only the toluene seems cloudy.

Should I pour all the contents to the dish or just one layer (and if so, which one)? The Tek does not specify so I poured all the contents to the dish.

Now the toluene formed cloudy "lakes" on the bottom of the dish.

I waited for an hour but no crystals appear.

My best bet is to separate the top layer (methanol?) and let the bottom layer slowly evaporate. Maybe the fumaric acid dissolves in methanol while the mecaline fumarate stays in the toluene (?)

Please advice, I don't want to lose almost half a gram of mescaline

 

[Mindlusion]

methanol isn't the best choice for fumaric salt precipitation because it dissolves alkaloid salts relatively well compared to other alcohols.

Still it should work, methanol isn't that soluble in toluene but my guess is that you have some water in your methanol and that is keeping everything dissolved in the methanol layer.

Toluene can take up quite a bit of water too (and it will look cloudy when wet), you should evaporate the whole thing and dry it if you want to recover everything

 

[blue.magic]

I am surprised the tek made it to the wiki :surprised . Shouldn't it be updated with a more suitable chemicals then? What acid/solvents should then be used? I would try 69ron's d-limonene tek but I don't have access to d-limonene now, hence I tried Kash's tek as it looked straightforward - now I realize it's not that good.

The methanol gets inevitably in contact with water in the process so I can't imagine any way of taking it out dry.

It is also possible there is no actual mescaline in the extract but I already see some specks at the walls of the dish.

Maybe it's better to separate the layers and evaporate each seaparately? I guess the toluene layer will contain most of the mescaline fumarate while the methanol layer mostly the fumaric acid.

My goal is to roughly determine how much mescaline is in the extract so I can dose properly, that's the reason for purification.

 

[Mindlusion]

I am surprised the tek made it the the Wiki when there are good reasons not to recommend the purification. Shouldn't it be updated with a more suitable chemicals then? What acid/solvents should then be used? I would try 69ron's d-limonene tek but I don't have access to d-limonene now, hence I tried Kash's tek as it looked straightforward - now I realize it's not that good.

The methanol gets inevitably in contact with water in the process so I can't imagine any way of taking it out dry.

It is also possible there is no actual mescaline in the extract but I already see some specks at the walls of the dish.

Maybe it's better to separate the layers and evaporate each seaparately? I guess the toluene layer will contain most of the mescaline fumarate while the methanol layer mostly the fumaric acid.

My goal is to roughly determine how much mescaline is in the extract so I can dose properly, that's the reason for purification.

No, the purification works fine, i've used methanol before, it is just not my first choice, it does have its advantages..

The methanol gets inevitably in contact with water in the process so I can't imagine any way of taking it out dry.

Huh? When? Taking it out of the bottle?

Maybe it's better to separate the layers and evaporate each seaparately? I guess the toluene layer will contain most of the mescaline fumarate while the methanol layer mostly the fumaric acid.

No, it will be primarily in the water/methanol layer. You could separate if you want but you should then also wash the toluene with water and collect the water layers, to avoid losses. Or simply evaporate all of it and repeat the procedure with a little more attention to detail.

Mind you, im not sure how impure your extract is, it can be very difficult to crystallize alkaloid salts by this method if the sample is impure, no matter the water content

I would try 69ron's d-limonene tek but I don't have access to d-limonene now, hence I tried Kash's tek as it looked straightforward - now I realize it's not that good.

the non-polar solvent won't make a difference, before you go changing things arbitrarily try to figure out what went wrong rather than blaming the technique..

for one, it looks like you used way too much methanol/fumaric acid.... one of the advantages of methanol is that fumaric acid is much more soluble in it, so you only need to add a few drops to the non-polar, that solves the issue of increased solubility, especially with larger amounts..

 

[blue.magic]

Huh? When? Taking it out of the bottle?

Step 2. of the Kash's purification Tek. In step 2. it says to add toluene to the water solution:

1. To a glass container with 1g cleaned Mescaline Hcl add 50ml H2O + 1ml HCl. Mix well until crystals completely dissolve.
2. Add 50ml toluene.
3. Mix 10g NaOH with 50ml water and add this to the solution, turning it basic. Mix well for 10 minutes.
4. Seperate layers, saving toluene and discarding aqueous.

He even advices to mix it for 10 minues. In step 4. the toluene layer is separated. I've used pipette and made sure there is only one layer - I don't see any water other than supposedly dissolved in the toluene.

before you go changing things arbitrarily, try to figure out what went wrong rather than blaming the technique

I admit. I was angry because I followed the steps to the letter then doomed to lose the expensive product. I even use pure lab chemicals, measure everything to 0.5ml or milligram precision so I don't know what could possibly went wrong. Hence the reaction...

Anyway - I evaporated the layers. The methanol layer is on the left, toluene layer on the right.

for one, it looks like you used way too much methanol/fumaric acid.... one of the advantages of methanol is that fumaric acid is much more soluble in it, so you only need to add a few drops to the non-polar, that solves the issue of increased solubility, especially with larger amounts..

I don't know how to determine how much to use. I used the number from the Tek scaled to the amount of extract I used.

I cannot guess how much mescaline is there. That's why I am doing purification in the first place.

 

[Mindlusion]

Huh? When? Taking it out of the bottle?

Step 2. of the Kash's purification Tek. In step 2. it says to add toluene to the water solution

I was talking about water in methanol, i mentioned toluene but i shouldn't have confused you , its negligible.

--

looks like you have a lot of excess fumaric acid, the toluene had some methanol dissolved so it gave some crystals too, i would combine them both and do a clean up. Don't use so much methanol/fumaric acid

 

[Mindlusion]

I don't know how to determine how much to use. I used the number from the Tek scaled to the amount of extract I used.

I cannot guess how much mescaline is there. That's why I am doing purification in the first place.

there is kind of a feel for it, I usually just add it dropwise until I no longer see any clouding. Sometimes this isn't enough, you can always use pH papers.

but to me it looks like you didn't add twice as much more like 5x or 10x as much

 

[blue.magic]

The tek calls for 0.5g fumaric acid for 1g of extract.

Since I have 0.389g extract, I've used about 0.194g of fumaric acid. It's just a speck. That's still too much?

What you see on the dish is certainly not a fumaric acid. I have not used that much. It was like a few grains of salt or so...

 

[Mindlusion]

The tek calls for 0.5g fumaric acid for 1g of extract.

Since I have 0.389g extract, I've used about 194 milligrams of fumaric acid. It's just a speck. That's still too much? I had to use milligram scale to measure it properly.

What you see on the dish is certainly not a fumaric acid. I have not used that much. It was like a few grains of salt or so...

I would use less but how do I know that's enough? Or that's too little?

Maybe by adding fumaric acid solution slowly until no clouds appear?

Ok then maybe it looks better than I thought, you didn't use too much fumaric just too much methanol.

it could be mostly mescaline fumarate, im not sure on the solubility of that salt, but if it follows the trend you could dissolve it in a minute amount of water and pour it off from excess fumaric acid/evap impurities into a little shot glass and let it evap slow to form pure crystals

 

[blue.magic]

you could dissolve it in a minute amount of water and pour it off from excess fumaric acid/evap impurities into a little shot glass and let it evap slow to form pure crystals

Okay but some crystal washing need to be done as the impurities settle on top of the crystals anyway, right?


How do you guess the amount of methanol? Is there any formula for it? I can learn molar counts if that is necessary but I hoped it's not that complicated.

 

[Mindlusion]

you could dissolve it in a minute amount of water and pour it off from excess fumaric acid/evap impurities into a little shot glass and let it evap slow to form pure crystals

Okay but some crystal washing need to be done as the impurities settle on top of the crystals anyway, right?


How do you guess the amount of methanol? Is there any formula for it? I can learn molar counts if that is necessary but I hoped it's not that complicated.

saturate the methanol with fumaric acid, it takes a while to dissolve but methanol will dissolve more than ethanol, acetone or ipa. I use a microwave to speed things up (not for food lab use only). Then I just store this solution for when I need it.

you may or may not need to wash them, just decant it from the insolubles, put a piece of Al foil over the glass (loosely) or paper towel to keep dust out. But a quick rinse with acetone at the end never hurts, also it helps the crystals dry faster

 

[blue.magic]

Thanks for all the advice.

I have finally collected 263 mg of powder of which 194 mg should be the fumaric acid. So 69 mg of mescaline at best (from two 12" San Pedros) - probably more like 50 mg or so...

It seems the amount of mescaline is sub-threshold and it won't have any effect.

I will study forums for different advice to improve the mescaline extraction later. It seems it has many cuplrits that are not described in a single Tek and one has to experiment a lot before getting grip of it.

 

[urtica]

Do you know what type of San Pedro you were using? There are many species and clones, some of which are alkaloid rich and some of which don't have much alkaloids in them at all.

 

[blue.magic]

It was a San Pedro cutting cultivated in Europe so maybe the low alkaloid content is due to it growing in greenhouse conditions instead of wildly.

I don't know about the sub-species (see the photo).

Maybe it's more viable to extract from powder originating in South America rather than from living cacti.

 

[blue.magic]

methanol isn't the best choice for fumaric salt precipitation because it dissolves alkaloid salts relatively well compared to other alcohols.

What solvent would you use then? Acetone?

 

[endlessness]

Yes, acetone or IPA work much better for fumaric salt precipitation

 

[downwardsfromzero]

Maybe it's more viable to extract from powder originating in South America rather than from living cacti.

I can wholeheartedly assure you, it is possible to grow potent SP in pots in Europe.

 

[blue.magic]

Maybe it's more viable to extract from powder originating in South America rather than from living cacti.

I can wholeheartedly assure you, it is possible to grow potent SP in pots in Europe.

It's good to know

Okay, so it was either the cacti specimen being too weak or I did something wrong in the extraction (more likely).

I remember I added a DCM defatting step - maybe that could have removed some mescaline from the acidic solution? The Tek does not have a defatting step but I though it would be nice for easier separation and less emulsion (some other sources include defatting though with xylene, not DCM - but any traditional nonpolar solvent would work, right?)

The solution was slightly acidic (citric acid used) and maybe some alkaloids were removed with the fats during defatting (e.g. trapped in fat droplets maybe, I don't know)...

Anyway, I will try next time without defatting and refreeze the cubed cacti (I forgot this step though I cooked/cloth-filtered it really thoroughly several times).

 

[Mindlusion]

Maybe it's more viable to extract from powder originating in South America rather than from living cacti.

I can wholeheartedly assure you, it is possible to grow potent SP in pots in Europe.

It's good to know

Okay, so it was either the cacti specimen being too weak or I did something wrong in the extraction (more likely).

I remember I added a DCM defatting step - maybe that could have removed some mescaline from the acidic solution? The Tek does not have a defatting step but I though it would be nice for easier separation and less emulsion (some other sources include defatting though with xylene, not DCM - but any traditional nonpolar solvent would work, right?)

The solution was slightly acidic (citric acid used) and maybe some alkaloids were removed with the fats during defatting (e.g. trapped in fat droplets maybe, I don't know)...

Anyway, I will try next time without defatting and refreeze the cubed cacti (I forgot this step though I cooked/cloth-filtered it really thoroughly several times).

In my experience mescaline salts are quite soluble in DCM, even sulfate, I had almost 1g of mescaline sulfate dissolved in 50mL of DCM at room temp, which later crystallized out in the freezer.. However once it crystallizes out it is impossible to get it back into the same solution

Still salts will perfer the aqueous phase, but defat with DCM might not be a good idea unless you back extract the defats too with acidic water

 

[blue.magic]

I see. No more DCM then. From what I read on forums, the cactus fats are not that big issue anyway.

...so to remove excess fumaric acid, I used the "shotglass" method - redissolved the ~260 mg of extract in clean anh. acetone, mixed well, let the insolubles sit, decanted the acetone, dried and obtained ~120 mg of what I believe is mostly mescaline fumarate.

I will try this some day to check whether it has at least mild threshold effects. I believe the amount of remaining fumaric adic is non-toxic.