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Defatting IS necessary even with alcoholic extraction
- Thread starter blue.magic
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blue.magic
Esteemed member
Jees said:
Yes that happened to me too. Washing the solvent with water caused noticeable loss of yield.
Now I prefer to dry the xylene pulls with calcium chloride to remove basic water and water-soluble impurities, before backsalting into distilled water.
Jees said:
The salt seems to really like to stay in polar solvent, which explains why backsalting works so well and just one pull is needed.
The freebase is still "moderately soluble" in water though which in several gram scale can cause a substantial loss of yield.
pete666 said:
I was talking about A/B extraction - whether using just enough acid to get pH 4.0 and then just enough base to get pH 10.0 will suffice, or whether pushing the pH range (i.e. using loads of acid and loads of base) has any added benefit (e.g. getting rid of some organic impurities).
pete666 said:
It seems fine (see image). I have just added xylene to the sample of acidic mother liquor and shook it quite vigorously. The layers separated very quickly. There are some minor bubbly "clouds" but I know these go away quite easily with the aid of heat and stirring.
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blue.magic said:
My last A/B was many years ago (yes, i am using just STB), so I can't speak from experience. But I would say as far as pH is OK to keep the alkaloids in fb or salt form, it is not necessary to push it further.
blue.magic said:
Lovely
Was the liquor from whole cactus?
blue.magic
Esteemed member
pete666 said:
Everything except the core.
I will continue today with extraction - hoping for salvaging some mesc :roll:
blue.magic
Esteemed member
I have heated the acidic solution to 35-40 °C and de-fatted with 100 ml xylene four times. This was very easy.
I then added 50% NaOH solution in small portions while mixing. To my surprise, the mobile brown liquid turned into somewhat thicker dark green syrupy liquid with foam on top:
The pH was already 10, but I added excess base just to see whether the foam will go away (in fear of more emulsions). With excess base, the foam finally succumbed:
Unfortunately, the emulsion got even worse than last time. Even excessive heating and stirring (plus added salt) over two hours have not resolved even a tiny bit:
There is either much more fats in the cactus that more thorough de-fatting is needed, or some other emulsifier substance that works in basic environment (saponified fats?).
I will drain ass much water as possible and then capture it with calcium chloride, filter and proceed with backsalting. I am curious whether emulsions will still happen after de-fatting.
Maybe adding only necessary amount of dilute base would work better - possibly weaker base such as aqueous ammonia might work better than NaOH.
I then added 50% NaOH solution in small portions while mixing. To my surprise, the mobile brown liquid turned into somewhat thicker dark green syrupy liquid with foam on top:
The pH was already 10, but I added excess base just to see whether the foam will go away (in fear of more emulsions). With excess base, the foam finally succumbed:
Unfortunately, the emulsion got even worse than last time. Even excessive heating and stirring (plus added salt) over two hours have not resolved even a tiny bit:
There is either much more fats in the cactus that more thorough de-fatting is needed, or some other emulsifier substance that works in basic environment (saponified fats?).
I will drain ass much water as possible and then capture it with calcium chloride, filter and proceed with backsalting. I am curious whether emulsions will still happen after de-fatting.
Maybe adding only necessary amount of dilute base would work better - possibly weaker base such as aqueous ammonia might work better than NaOH.
Well, the gods are not giving it for free. Very bad news I would say.
Just one thing...have you added the salt before you got into troubles or afterwards? If before, you can try it without it. I am saying that, because I was trying to use it in dmt STB and got one of the most resistant emulsions I had ever seen. Therefore I never use salt for dmt STB. There is no need for salt and I am not experiencing emulsions anyway.
But for mescaline I had never such troubles, in fact it helps me to beat emulsion which I always have if not using it. Again, this is true for green tissue only.
Just one thing...have you added the salt before you got into troubles or afterwards? If before, you can try it without it. I am saying that, because I was trying to use it in dmt STB and got one of the most resistant emulsions I had ever seen. Therefore I never use salt for dmt STB. There is no need for salt and I am not experiencing emulsions anyway.
But for mescaline I had never such troubles, in fact it helps me to beat emulsion which I always have if not using it. Again, this is true for green tissue only.
blue.magic
Esteemed member
I tried both with salt and without. Unfortunately, there are already salts present from the neutralization when re-acidifying the mother liquor.
Here is the follow-up:
The emulsion occured again with the same vigor. Now I know it's something in the cactus. I have a strong feeling this is caused by powder from my own dried cactus:
I transfered the pulls + emulsion into an Erlenmeyer flask, added copious amount of calcium chloride and swirled. The emulsion broke down immediately and brown sludge settled on bottom.
I then vacuum-filtered everything. The sludge did not come through even on full vacuum. However, something interesting happened. You can see a hard calcium chloride cake with the sludge on top, which resembles a melted chocolate. This oily stuff is probably what causes all the trouble:
There were virtually no alkaloids in the filtered xylene but at least the layers separated easily and cleanly even after vigorous shaking.
Lessons learned:
- keep concentration low, use up to 200 g cactus powder per 1L alcohol or water, not more; do more runs if processing more material
- use more acid (won't hurt and possibly breaks down stuff)
- be careful about the base, use dilute base and use just enough to reach pH 8-10 and add it slowly with stirring
- use xylene instead of toluene
- do not wash solvent with water
Here is the follow-up:
The emulsion occured again with the same vigor. Now I know it's something in the cactus. I have a strong feeling this is caused by powder from my own dried cactus:
I transfered the pulls + emulsion into an Erlenmeyer flask, added copious amount of calcium chloride and swirled. The emulsion broke down immediately and brown sludge settled on bottom.
I then vacuum-filtered everything. The sludge did not come through even on full vacuum. However, something interesting happened. You can see a hard calcium chloride cake with the sludge on top, which resembles a melted chocolate. This oily stuff is probably what causes all the trouble:
There were virtually no alkaloids in the filtered xylene but at least the layers separated easily and cleanly even after vigorous shaking.
Lessons learned:
- keep concentration low, use up to 200 g cactus powder per 1L alcohol or water, not more; do more runs if processing more material
- use more acid (won't hurt and possibly breaks down stuff)
- be careful about the base, use dilute base and use just enough to reach pH 8-10 and add it slowly with stirring
- use xylene instead of toluene
- do not wash solvent with water
blue.magic
Esteemed member
Yes this time I will deskin the cacti and perform the defat right away; also being more careful about the use of acid and base - and praying to Mescalito in the process 
... I will post the results then.
... I will post the results then.blue.magic said:Yes this time I will deskin the cacti and perform the defat right away; also being more careful about the use of acid and base - and praying to Mescalito in the process
Honestly, deep communication with those guarding the power seems to help a lot with our endeavours...
blue.magic
Esteemed member
I ended up with 0.86 g of crude sulfates from 38 g of wachuma powder made from dethorned, despined and deskinned cacti.
The crude yield is thus 2.26%, which corresponds to the amount of powder used and the fact the powder was stronger than average.
The emulsion still occurred though it wasn't as bad as earlier. I found density is a big factor in emulsion breaking (salt or amount of base had no effect on it, but diluting the tea a bit allowed the liquid to separate better - this makes sense as bubbles in thick syrup won't go away easily).
What also occurred was the oily "chocolate" layer. I extracted it and it have not contained alkaloids, which is a good news. This meands emulsion can be killed with drying agent and the solvent decanted from the oil/desiccant suspension.
This time no emulsion happed in the final backsalting, even if shaken like crazy. It seems adding somewhat dilute base while strongly stirring is beneficial. Using xylene over toluene can be another reason.
Foolish me I haven't done the defatting. I wait for wachuma from Peru, enough for thorough experimentation. I will then try the defatting approach.
The crude yield is thus 2.26%, which corresponds to the amount of powder used and the fact the powder was stronger than average.
The emulsion still occurred though it wasn't as bad as earlier. I found density is a big factor in emulsion breaking (salt or amount of base had no effect on it, but diluting the tea a bit allowed the liquid to separate better - this makes sense as bubbles in thick syrup won't go away easily).
What also occurred was the oily "chocolate" layer. I extracted it and it have not contained alkaloids, which is a good news. This meands emulsion can be killed with drying agent and the solvent decanted from the oil/desiccant suspension.
This time no emulsion happed in the final backsalting, even if shaken like crazy. It seems adding somewhat dilute base while strongly stirring is beneficial. Using xylene over toluene can be another reason.
Foolish me I haven't done the defatting. I wait for wachuma from Peru, enough for thorough experimentation. I will then try the defatting approach.
I am suspecting the amount of water to be directly correlated to the emulsion too. The only problem is the predicate, that the more water there is, the less mescaline is transfered to non-polar solvent. I am planning to do some tests with these variables, so we know where we are. Fortunately my emulsion tests didn't use too much material, so I have enough to test other ideas.
blue.magic
Esteemed member
Yes I have just read that in one of your recent posts.
Knowing the mescaline solubility in various solvents would be helpful.
I am thinking about modeling the amount of mescaline extracted given the amount of tea, density/viscosity, amount of solvent and number of pulls.
I am thinking about reusing the solvent after backsalting for another extraction followed by backsalting. This way we can assess how efficient the solvent is. Actually backsalting every pull separately will give a curve from which we can calculate the relative solubility of mescaline in the given solvent vs. mother liquor.
Calculating the viscosity is harder but maybe density of the mother liquor could be used as a measure for obtaining just the right concentration to avoid emulsions.
I will also try to compare the results with and without de-fatting.
Last idea I had, but this is relevant only to A/B, not STB, is that adding base to possibly highly acidic tea will produce some salt, increasing the chance for emulsion. But this is gram amounts and may not be significant. I will anyway try to use only minimal amount of acid (pH 6 is more than enough to salt virtually all of the mescaline - last time I got pH 0.5 - way too much acid has been used).
Knowing the mescaline solubility in various solvents would be helpful.
I am thinking about modeling the amount of mescaline extracted given the amount of tea, density/viscosity, amount of solvent and number of pulls.
I am thinking about reusing the solvent after backsalting for another extraction followed by backsalting. This way we can assess how efficient the solvent is. Actually backsalting every pull separately will give a curve from which we can calculate the relative solubility of mescaline in the given solvent vs. mother liquor.
Calculating the viscosity is harder but maybe density of the mother liquor could be used as a measure for obtaining just the right concentration to avoid emulsions.
I will also try to compare the results with and without de-fatting.
Last idea I had, but this is relevant only to A/B, not STB, is that adding base to possibly highly acidic tea will produce some salt, increasing the chance for emulsion. But this is gram amounts and may not be significant. I will anyway try to use only minimal amount of acid (pH 6 is more than enough to salt virtually all of the mescaline - last time I got pH 0.5 - way too much acid has been used).
This is what I am doing in every extractionblue.magic said:
For this STB I get (just one extraction) :
1. pull 68% (4.909g) of mescaline
2. pull 22% (1.667g) of mescaline
3. pull 11% (0.813g) of mescaline
I am not sure how to say how much mescaline remained in the water, but I would say not much. The water was fully saturated by NaCl though
I am planning to do parallel extractions of known material with various amounts of water and see the impact of water volume on the yield
Anyway, I understand your drive to continue with this method, but you might consider partaking in the STB TEK I am trying. Last tests look very promising and I believe more people can make it reliable non-emulsion TEK rather than one.
blue.magic
Esteemed member
Thanks for the data.
I will probably do both Teks and compare the results (yield, relative purity via TLC, reagent cost, labour cost). Competition is a driving force for innovation anyway
If oils are the main cause of emulsions, it could be a bigger obstacle to design a versatile STB Tek, as particularly high-fat cacti might be prone to saponification and subsequent emulsification. But I will sacrifice up to 200 g of wachuma powder for this research.
I will probably do both Teks and compare the results (yield, relative purity via TLC, reagent cost, labour cost). Competition is a driving force for innovation anyway
If oils are the main cause of emulsions, it could be a bigger obstacle to design a versatile STB Tek, as particularly high-fat cacti might be prone to saponification and subsequent emulsification. But I will sacrifice up to 200 g of wachuma powder for this research.
Makes sense.
My feeling is there is something else than just oils causing saponification with high pH. But this is just a feeling
I believe there are more various emulsions in the game, some stable and some unstable. I have never seen stable emulsion without NaCl for mescaline. But without NaCl there is always unstable emulsion, hour or two of heating leads to its decomposition.
With NaCl, there was ugly stable emulsion, and stable means stable. No known method leads to its decomposition.
So the main aim is to use NaCl to avoid unstable emulsion and find way how to avoid the stable one. If there is no way of avoiding it, then identify for what cactus or/and part it happens and avoid using the TEK for it.
How are you processing TLC? With endlessness?
My feeling is there is something else than just oils causing saponification with high pH. But this is just a feeling
I believe there are more various emulsions in the game, some stable and some unstable. I have never seen stable emulsion without NaCl for mescaline. But without NaCl there is always unstable emulsion, hour or two of heating leads to its decomposition.
With NaCl, there was ugly stable emulsion, and stable means stable. No known method leads to its decomposition.
So the main aim is to use NaCl to avoid unstable emulsion and find way how to avoid the stable one. If there is no way of avoiding it, then identify for what cactus or/and part it happens and avoid using the TEK for it.
How are you processing TLC? With endlessness?
downwardsfromzero
Boundary condition
There are so many things in cactus flesh that could cause emulsions. Even some of the phenolic alkaloids could do so at high pH. Then there's chorophyll breakdown products, possibly a selection of phenolic flavonoids, and peptides of various sizes, not to mention the polysaccharide gloop.
Contrasting the stability of the NaCl emulsion with the instability of the emulsion without NaCl must in some way inform us of the culprits - substances forced out of solution by higher ionic strength? That could be any of them, really.
Incidentally, given that we can fairly confidently consider flavonoids to be responsible for the enhanced potency of T. bridgesii, it's arguably a good idea to use more complete extracts from that species rather than going for pure mescaline and the attendant risk of emulsion nightmares!
Contrasting the stability of the NaCl emulsion with the instability of the emulsion without NaCl must in some way inform us of the culprits - substances forced out of solution by higher ionic strength? That could be any of them, really.
Incidentally, given that we can fairly confidently consider flavonoids to be responsible for the enhanced potency of T. bridgesii, it's arguably a good idea to use more complete extracts from that species rather than going for pure mescaline and the attendant risk of emulsion nightmares!
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