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Cactus soxhlet extraction ideas

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ThirdEyeVision

ThirdEyeVision

Rising Star
My friend is looking for a reliable way to use a soxhlet with cactus powder. Very little info was found on the web regarding soxhlet and cacti. I did see where 69Ron's friend had poor luck with both IPA and Methanol on cactus in it's natural form, assuming from heat.

1) After reading 69Rons post on the characteristics of different mescaline forms I see freebase boils at about 35c but hydrochloride boils at 184c. Does that mean as a hydrochloride the mescaline should be relatively safe at 79c?

2) If it is safe at 79c couldn't one make a paste from cactus powder by adding diluted hydrochloric acid to convert the natural mecaline salt to a
hydrochloride?

3) If that would succesfully convert to a hydrochloride, could one then dry and extract with a soxhlet using denatured ethanol at 79c without significant degrading?

If my thinking is wrong, any other ideas?
 
Why not incorporate the acid in the soxhlet solvent employing acidified alcohol,or measuring the volume free in the flask and prewetting the cacti to be extracted in the thimble with HCl solution that will not overfill the flask beyond its capacity?


Also: Are we sure that mescaline exists as freebase in the cactus? One could expect it to be able to come in contact with plant acids...
 
Crystalito said:
Why not incorporate the acid in the soxhlet solvent employing acidified alcohol,or measuring the volume free in the flask and prewetting the cacti to be extracted in the thimble with HCl solution that will not overfill the flask beyond its capacity?


Also: Are we sure that mescaline exists as freebase in the cactus? One could expect it to be able to come in contact with plant acids...
Click to expand...
My friend is very new to the soxhlet so not sure what the best way would be. He assumed the acid wouldn't distill making it not work in the soxhlet. That is just a assumtion though.

I couldn't find anywhere how it naturally exists in the cacti.
 
SWIM is wondering the same thing! - Please help someone!
What is the best solvent to use in the soxhlet for mescaline?
Does the cactus matter need to be dry and powdered or can it be wet and blended?
Would vinegar be safe to use as the added acid?

cheers
 
My friend has a plan, please tell me what you think of it:
1) Put dried cactus in blender with Calcium hydroxide.
2) Mix resulting powder with just enough water to make paste.
3) Let dry over night.
4) Pour powder into soxhlet.
5) Extract with DCM overnight(for it's very low boiling point of 104f)


That should work thus far, right?
Could he then convert the mescaline freebase to acetate by mixing the DCM with viniger in a seperatory funnel and seperating out the DCM and evaping the viniger?
 
ethanol pulls aLot of crap besides mescaline from the cacti, which is ok, but requires further purification down the road.

you wont find much on this type of extraction on the net because it is not terribly practical
 
ThirdEyeVision: I know this is old, but how did it go? Did it work? Was the ethanol acidified? I was wondering the same thing about HCl not being distilled along with the ethanol.
 
My mathematician friend conducted a simple experiment very relevant to the discussion:

He added 0.5ml conc. HCl to 150ml ethanol 96% (pH 7.82), resulting in a solution of pH 0.7. He then brought it to a boil in a soxhlet, allowed one cycle to take place, and then stopped the heating in the middle of the second cycle. He allowed the apparatus to reach room-temperature and measured the pH of the solution in the extraction vessel to be 7.7. The liquid remaining in the heating vessel had a pH of 0.62.

He concluded that acidifying ethanol with HCl for a soxhlet extraction does not work as one would desire, at least with the composition mentioned above. One should use the azeotropic mixture of the system ethanol/water/HCl for this to work. If somebody has access to it, post it here. He thinks that soaking the material in ethanol/HCl prior to the extraction could help.
 
After further experimentation, she reports that a solution of ethanol/water/HCl in the proportions 90/10/1 v/v/v is what somebody desiring to perform a soxhlet extraction on cactus material is looking for. The distillate in the soxhlet vessel has a pH of ~3, and the solution in the heating vessel a pH of ~0.5.

She is quite happy with the results. More information can be found in this paper: Amino and Fatty Acids of Wild Edible Mushrooms of the Genus Boletus, Dembitsky (2010).
 
Adivino said:
ThirdEyeVision: I know this is old, but how did it go? Did it work? Was the ethanol acidified? I was wondering the same thing about HCl not being distilled along with the ethanol.
Click to expand...

low grade ethanol(drinkable proof) doesn't need to be acidified to pull cacti alkaloids, they are plenty soluble in polar solvents as is
 
dg said:
Adivino said:
ThirdEyeVision: I know this is old, but how did it go? Did it work? Was the ethanol acidified? I was wondering the same thing about HCl not being distilled along with the ethanol.
Click to expand...

low grade ethanol(drinkable proof) doesn't need to be acidified to pull cacti alkaloids, they are plenty soluble in polar solvents as is
Click to expand...

So would you think a cheap vodka (35-40%) would work fairly well on its own in a soxhlet? Then maybe run it through a filter with a tbs or so of activated carbon to remove some of the impurities pulled?
 
So would you think a cheap vodka (35-40%) would work fairly well on its own in a soxhlet? Then maybe run it through a filter with a tbs or so of activated carbon to remove some of the impurities pulled?
Click to expand...

I think that 35-40% ethanol will distill slowly because of the big amount of water. Also, since this behaves like simple distillation, the concentration of ethanol in the vapor (and therefore condensation) will not be the highest (azeotropic) one. This means that the cactus cells could swell because of the condensed water.

If you can, try to run the soxhlet using the azeotropic mixture detailed above of ethanol:water:HCl 90:10:1 (v:v:v). Even though there's some water here, it's presence is crucial for the HCl to distill over (experiments without the water resulted in a neutral pH in the extraction vessel (where the plant material is)).

This looks promising. I'll try to do it (for the sake of science) when I have the time.
 
Attention All Shipping, extraction with azeotropic ethanol/HCl/water is too unspecific and results in a brown oily ethanolic solution. This is acceptable if your goal is the resin, but I'd use only ethanol 96-98% if I was planning to do an A/B extraction.
 
ThirdEyeVision said:
My friend has a plan, please tell me what you think of it:
1) Put dried cactus in blender with Calcium hydroxide.
2) Mix resulting powder with just enough water to make paste.
3) Let dry over night.
4) Pour powder into soxhlet.
5) Extract with DCM overnight(for it's very low boiling point of 104f)


That should work thus far, right?
Could he then convert the mescaline freebase to acetate by mixing the DCM with viniger in a seperatory funnel and seperating out the DCM and evaping the viniger?
Click to expand...

This works with limo and day long pulls instead of a solhext ime (drying lime/cactus powder paste then decanting/pouring off the limo). I'd love to see someone try it with alcohol or dcm, etc and using a solhext. Basing the powder first just makes more sense in that it breaks down the cells to a degree, and mesc fb is much more soluble in alcohols than hcls.

Of course with more NP solvents like dcm and limo you have to base first, but it seems like a good idea for a mesc extraction, or at least an improvement over straight alcohol soak crude extractions.
 
Adivino said:
Attention All Shipping, extraction with azeotropic ethanol/HCl/water is too unspecific and results in a brown oily ethanolic solution. This is acceptable if your goal is the resin, but I'd use only ethanol 96-98% if I was planning to do an A/B extraction.
Click to expand...

I'm currently soaking some cactus powder in 96% alcohol for extraction of resin, after that pull I considering putting it in a soxhlet to see how much else can be extracted.
I've been reading up on A/B for mescaline, not sure how it'd work with A/B on alcohol - would it operate the same way to limonene/xylene?
 
You have to completely evaporate the alcohol to obtain a solid mass, which is then dissolved in (warm) water, basified and extracted with a non-polar solvent. You may want to defat first, since it's very probable that the alcohol extract will contain plant lipids, which will otherwise dissolve in the non-polar solvent, together with some desired alkaloid.
 
Tried a soxhlet extraction with ethanol, but with no success. There was just no drainage of liquid through the cactus powder (pre-wetted) and it got clogged.

How do you guys ensure good drainage & functioning soxhlet with cactus powder?
 
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