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Kash's A/B Mescaline Extraction

Migrated topic.
I think the order you added your material played a larger issue... Take your plant material and add it to the alkaline NaOH solution. Add enough water that you can swirl that plant material and it doesn't just form a mass.

I usually leave this in the strong lye solution for a day before added the xylene to begin pulling.... Since you have an Ultrasonic you can probably just leave the lye cactus solution for say an hour before adding the xylene.

After adding the xylene I always shake the two layers but most suggest just swirling... At this point I'd suggest adding salt until saturation. This works for two purposes to change ionic strength and prevents/reduces emulsions by making a higher polarity thus better better separation with the solvent.

IF you still have an emulsion I'd suggest adding more solvent... I think think an ultrasonic bath of the solvent and lye solution is a good idea compared to just shaking the two? IDK but you want the most contact of the two.

EDIT: Are you sure you have the correct cactus materiel?
 
Thank you all, you folk are awesome.

I jumped in to this before getting the theory in, and I really should've read some forums too.
I've now got the book https://www.amazon.ca/Solvent-Extraction-Principles-Practice-Expanded/dp/0367578417/ for the theory. Are there any other books anyone can recommend?

modern said:
EDIT: Are you sure you have the correct cactus materiel?
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The only way for me to know for sure is via consumption of it, but the source of the seeds indicated it was.

modern said:
At this point I'd suggest adding salt until saturation.
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We're talking sodium chloride, and saturation would be where the salt crystals do not dissolve?
doubledog said:
Main mistake was discarding cactus material after first unsuccessful attempt. ;)
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The cactus material still contained a significant amount of xylene, which could not be further separated without additional chemicals. Should I have added the cactus mixture to a new, larger lye solution or done some preprocessing? My disposal method was incineration, which smoked intensely, resembling burning tire.

Originally, the mixture was a large, jelly-like blob that I couldn't remove from the flask. I had to heat it for a while, allowing it to slowly ooze out.

Thanks :)
 
Jelly-like blob indicates that cactus mucilage was not hydrolysed enough to release mescaline freebase into xylene. It would needed just to add some water and maybe NaOH, wait 2 days and repeat extraction multiple times (but with less xylene for each cycle).

You probably incinerated two or three grams, maybe even more, of mescaline. :(
 
JackAllMasterNone said:
Thank you all, you folk are awesome.

I jumped in to this before getting the theory in, and I really should've read some forums too.
I've now got the book https://www.amazon.ca/Solvent-Extraction-Principles-Practice-Expanded/dp/0367578417/ for the theory. Are there any other books anyone can recommend?


The only way for me to know for sure is via consumption of it, but the source of the seeds indicated it was.


We're talking sodium chloride, and saturation would be where the salt crystals do not dissolve?

The cactus material still contained a significant amount of xylene, which could not be further separated without additional chemicals. Should I have added the cactus mixture to a new, larger lye solution or done some preprocessing? My disposal method was incineration, which smoked intensely, resembling burning tire.

Originally, the mixture was a large, jelly-like blob that I couldn't remove from the flask. I had to heat it for a while, allowing it to slowly ooze out.

Thanks :)
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You can add to complete saturation but depending on the volumes you are working with it will be a LOT of sodium chloride. I usually add to saturation but work with smaller volumes. Adding a 'fair' amount of salt will help regardless. Also the amount of lye changes the amount of salt needed compared to pure water. Salt is cheaper than lye in most cases. Try to use iodine free but doesn't matter much IME.

If you still have the cactus with the xylene you could have added a salt brine lye solution and leave it sitting for a few days. There is a tiny amount of loss of xylene I experience but mostly from the thin surface tension not the plant material. After extractions I tend to leave the cactus material for even longer with lye and salt and just leave some xylene in contact for another week or longer and pull again sometimes with minimal to no more alkaloids but since you are using large amount of material will be more worth while.
 
Trust me, I already feel bad about cutting down the 1750mm cactus and another 400mm one, just to waste it :(

How does the below tek + ratios look for a quick and ez to remember extraction?
Your first reaction will probably be, "why mess around with ultrasonics/sonochemistry when we already get good results?". In my experience extracting flavors and what not from botanicals is much improved with ultrasonics and in a fraction of the time, but the problem here is that it will even emulsify xylene with water without some form of preventative. A 2L 40kHz ultrasonic bath is ~$75.
But remember I have no idea what I am doing, and all I have behind me is one failed attempt after reading Kash's tek and thinking I could skip steps, and not even read about Solvent Extraction Principles... so the following is my next attempt plan.

Ingredients
  • 100 g dried cactus powder (devoid of waxy skin)
  • 1600 mL distilled water
  • 500 g sodium chloride (NaCl)
  • 100 g sodium hydroxide (NaOH)
  • 1000 mL xylene
  • 3 mL concentrated hydrochloric acid (HCl, 30% solution)
Apparatus
  • 3L borosilicate flask or beaker ($20)
  • 1L Separatory funnel ($30)
  • Magnetic stirrer with heating function ($40)
  • 28 kHz ultrasonic wand ($500) (optional).
  • Ultrasonic bath (adjustable frequency if possible) ($75-500)
  • Vacuum pump ($80) (optional)
  • pH strips
  • Syringe


Step 1: Prepare the Basic Solution and anti-emulsion.
  1. Add 1000 mL of distilled water to the 3L flask.
  2. Slowly add 100 g of NaOH to the water while stirring with a magnetic stirrer.
    • ** is this enough, Kash uses a 1:2 ratio vs 1:10?**.
    • Reaction will release heat; monitor temperature, which will rise to approximately 45°C.
  3. Gradually add 500 g of NaCl to the NaOH solution while continuing to stir.
    • Ensure all salt is fully dissolved or can't be dissolved further to create a saturated brine solution.

Step 2: Add Cactus Powder
  1. Slowly introduce 100 g of cactus powder into the flask while stirring continuously.
    • Maintain the stirrer speed at a "slow" setting to prevent excessive agitation but enough to incorporate everything.
  2. Immerse a 28 kHz ultrasonic wand into the mixture and ultrasonicate for 20 minutes while stirring or use a 40kHz ultrasonic bath for 3hrs on the highest setting.
    • Temperature will rise to approximately 55°C due to ultrasonic energy.
    • pH should remain above 13 due to the strong basicity of the solution.

Step 3: Introduce Xylene
  1. Slowly add 1000 mL of xylene to the mixture while stirring gently for 15 minutes.
    • Reduce stirring intensity to prevent excessive emulsification, but ensure the mixing looks homogenous.
    • Temperature will stabilize around 40°C.

Step 4: Ultrasonic Migration of Alkaloids
  1. Transfer the flask to a 80 kHz ultrasonic bath.
  2. Ultrasonicate the mixture for 1 hour on a low setting, maintaining a bath temperature of approximately 45°C.
    • This facilitates migration of alkaloids into the xylene phase.
    • This higher frequency promotes the coalescence of emulsified particles and better separation of phases. Think of it like a very gentle microscopic shaking.
Step 5: Separation of Phases
  1. Transfer the contents into a separatory funnel.
  2. Allow the mixture to settle until three distinct layers form:
    • Bottom layer: Dark aqueous solution containing NaOH, salt, and cactus solids (if present).
    • Middle layer: light green opaque fluffy cactus stuff.
    • Top layer: Xylene with the goodies.
  3. Decant the xylene layer (top) into a clean separatory funnel.
  4. Retain the bottom layer for additional xylene extractions, if desired or you fucked up somewhere and need to redo it.
Step 6: Acidification and Extraction
  1. Add 1 mL of concentrated (30%) HCl to 200 mL of distilled water in a container.
  2. Introduce the acidic water to 1/3 (330mL) the xylene and swirl well.
    • Mescaline freebase will convert into water-soluble mescaline hydrochloride and migrate to the aqueous layer.
  3. Allow the xylene and aqueous layers to separate.
  4. Decant the aqueous layer (now containing mescaline hydrochloride) into a separate container to evaporate, and put the xylene in another container for recycling.
  5. Repeat step 8 three times
But what about the waxy bubbles?
1735824392882.png
Step 7: Crystallization
  1. Evaporate the aqueous solution under vacuum or by gentle indirect heating to crystallize mescaline hydrochloride.
  2. Recrystallize/wash using Acetone Anhydrous for higher purity, if necessary.
 
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Some comments:

Step 3 and 4: use less xylene, 300ml or so and repeat this step few times. Mescaline freebase does not like to move into xylene very quickly, when dissolved in alkaline cactus soup. This is the main problem you have to adress with this style of extraction.

Step 5: Separatory funnel works well with liquids, better to not use it when cactus solids are there. Suck out xylene from the top and transfer to another container.
 
I suggest adding cactus to lye solution and ultrasound for an hour or so BEFORE adding your salt to make it a brine.

May not play a massive issue in practice but in theory the salt may compact the cells and keep mescaline trapped in the cells. The lye should break the cell and with ultrasonic more so.

With the waxy bubbles keep it with the xylene solution and seperate the water then shake/swirl and they should break. Add more xylene will break most emulsions. You can also do a salt brine wash to clean up the xyelne a bit and add a small amount of lye if you want.

If the bubbles are from the acid pulls DO NOT add salt wash. Either add more water or add more xylene. Swirl and let it break. You can also just add the bubbles to the acid water pulls and clean up and evaporate the small amount of xylene which always comes over.
 
doubledog said:
Step 3 and 4: use less xylene, 300ml or so and repeat this step few times. Mescaline freebase does not like to move into xylene very quickly, when dissolved in alkaline cactus soup. This is the main problem you have to adress with this style of extraction.

Step 5: Separatory funnel works well with liquids, better to not use it when cactus solids are there. Suck out xylene from the top and transfer to another container.
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If I am doing 3 x 300mL that would be almost 1L or do I remove any xylene at any point, or is it that I should just add the xylene in smaller amounts; I could even just drip it in over an hour if that's better?
Step 4 if the alkaloid doesn't migrate readily, do you think I should apply 40kHz ultrasonics for a long duration with intermittent resting and stirring?
modern said:
I suggest adding cactus to lye solution and ultrasound for an hour or so BEFORE adding your salt to make it a brine.

May not play a massive issue in practice but in theory the salt may compact the cells and keep mescaline trapped in the cells. The lye should break the cell and with ultrasonic more so.

With the waxy bubbles keep it with the xylene solution and seperate the water then shake/swirl and they should break. Add more xylene will break most emulsions. You can also do a salt brine wash to clean up the xyelne a bit and add a small amount of lye if you want.

If the bubbles are from the acid pulls DO NOT add salt wash. Either add more water or add more xylene. Swirl and let it break. You can also just add the bubbles to the acid water pulls and clean up and evaporate the small amount of xylene which always comes over.
Click to expand...
On my first attempt, shortly after adding the cactus powder to the lye solution, the blob formed. As I stirred, I could see it thickening, and once I stopped stirring, it congealed completely. I thought the xylene might break it down, and if that didn’t work, perhaps the ultrasonics would. However, the only thing that worked was applying heat to loosen the blob enough to remove it from the flask, followed by blending it on high.

Is there any method or process I can use to prevent the formation of emulsions when adding the powder to the lye solution? Would increasing the amount of lye help?

In step 6, adding more water didn’t help; the only effective solution was applying heat with a heat gun. The required heat was high enough to cause some water to boil, and the turbulence from boiling further broke the bubbles. After a few minutes, a thin white line formed, separating the xylene and water layers. When draining the separatory funnel, the white wax coated the glass. To clean the funnel, I rinsed it with isopropyl alcohol, which was very effective.

On the final evaporation step, I have the equipment for a vacuum evaporation, but how do I remove the formations from the boiling flask?

Thanks again and Happy New Year!
 
JackAllMasterNone said:
If I am doing 3 x 300mL that would be almost 1L or do I remove any xylene at any point, or is it that I should just add the xylene in smaller amounts; I could even just drip it in over an hour if that's better?
Step 4 if the alkaloid doesn't migrate readily, do you think I should apply 40kHz ultrasonics for a long duration with intermittent resting and stirring?

On my first attempt, shortly after adding the cactus powder to the lye solution, the blob formed. As I stirred, I could see it thickening, and once I stopped stirring, it congealed completely. I thought the xylene might break it down, and if that didn’t work, perhaps the ultrasonics would. However, the only thing that worked was applying heat to loosen the blob enough to remove it from the flask, followed by blending it on high.

Is there any method or process I can use to prevent the formation of emulsions when adding the powder to the lye solution? Would increasing the amount of lye help?

In step 6, adding more water didn’t help; the only effective solution was applying heat with a heat gun. The required heat was high enough to cause some water to boil, and the turbulence from boiling further broke the bubbles. After a few minutes, a thin white line formed, separating the xylene and water layers. When draining the separatory funnel, the white wax coated the glass. To clean the funnel, I rinsed it with isopropyl alcohol, which was very effective.

On the final evaporation step, I have the equipment for a vacuum evaporation, but how do I remove the formations from the boiling flask?

Thanks again and Happy New Year!
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Re the xylene volume - recycling one amount by salting between pulls would be a strategy to minimise the volume of NPS used. With this method it may be desirable to perform a quick treatment with sodium carbonate before returning the xylene to the basified plant mixture, depending on whether a significant excess of acid was used.

I've not done cactus/lye STBwith liquid-liquid extraction myself, but I've often seen it suggested that the answer to the gel situation is to add way more lye. The cactus mucilage is specifically made by the plant for holding onto loads of water and ions. Any slight kind of surfactant ability will cause to form impenetrable mayonnaise with a NPS, especial when it gets conveniently dispersed via ultrasound. Ergo, the more this mucilage gets hydrolysed by the lye, the better.

What precisely would your vacuum evaporation equipment be? A rotary evaporator would most conveniently be used with a pear-shaped flask which expedites the removal of solids with use of a spatula, but in all likelihood the simplest approach would be to dissolve out the solid with water and use a more open container (evaporaing basin, beaker, watch glass, glass petri dish, etc.) for recrystallising the product.
 
Based your feedback, I think I need to increase the lye from 100g to 250g and introduce the salt just prior to the xylene.
Transform said:
What precisely would your vacuum evaporation equipment be? A rotary evaporator would most conveniently be used with a pear-shaped flask which expedites the removal of solids with use of a spatula, but in all likelihood the simplest approach would be to dissolve out the solid with water and use a more open container (evaporaing basin, beaker, watch glass, glass petri dish, etc.) for recrystallising the product.
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I just use a hot plate magnetic stirrer, a vacuum pump and a Liebig condenser. I've got my eye out for a reasonably priced rotovap or might just make my own since I have all the parts except for a good way to connect the parts.
I usually stop the evaporation when the volume is near the bottom <100mL, and evap in a dish, but I know very few lab tricks.
 
JackAllMasterNone said:
Based your feedback, I think I need to increase the lye from 100g to 250g and introduce the salt just prior to the xylene.


I just use a hot plate magnetic stirrer, a vacuum pump and a Liebig condenser. I've got my eye out for a reasonably priced rotovap or might just make my own since I have all the parts except for a good way to connect the parts.
I usually stop the evaporation when the volume is near the bottom <100mL, and evap in a dish, but I know very few lab tricks.
Click to expand...
A pear-shaped flask would help there too. Pipetting out the last bit of liquid is a little easier that way. This talk of getting stuff out of flasks is making my OCD kick in :ROFLMAO:

Gradually adding more lye until the blob turns to liquid would appear to be the way. This may or may not turn out to be less than the increased amount you've suggest. Different plant specimens will have varying levels of mucilage, with varying degrees of resistance to hydrolysis.
 
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