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just wondering what solvents available in australia do people use on acacia phyllodes? does shellite usually suffice?
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A/B extraction on Acacia phyllodes
- Thread starter acacian
- Start date
What's the latest?
I was planning on doing a phyllode extraction on a untested acacia sp.
Here is how -
Boil phyllodes up with half ethanol, quarter filtered water, quarter vinegar, twice. Combine and reduce to 500ml.
Defeat once with xylene.
Basify with 100g sodium hydroxide.
Pull 3x with total 1 litre of xylene
Evap xylene for full spectrum extract.
I've got about 260g of dried phyllodes.
Does this sound okay?
Anyone got any improvements?
I was planning on doing a phyllode extraction on a untested acacia sp.
Here is how -
Boil phyllodes up with half ethanol, quarter filtered water, quarter vinegar, twice. Combine and reduce to 500ml.
Defeat once with xylene.
Basify with 100g sodium hydroxide.
Pull 3x with total 1 litre of xylene
Evap xylene for full spectrum extract.
I've got about 260g of dried phyllodes.
Does this sound okay?
Anyone got any improvements?
DreaMTripper
Rising Star
- Merits
- 42
Many reports of successful extractions start with a boiling of phyllodes in ethanol and water to extract the obstructive gums from the phyllodes. 70/30 should do it. Separate liquid from phyllodes and save this for a mini extraction afterwards.
Then proceed to boil phyllodes in solution that you mentioned however ethanol isnt neccessary now.
Instead of defatting you could just pull 4 times with 50-75ml of xylene (after base is added) then combine pulls.
Then back salt x5 with 50ml of vinegar.
Separate from xylene and put into a narrow bottle then basify with say 10g of lye or until pH 12-13. Add 100ml of salt saturated water.
Then pull x3 with 50ml of xylene and evaporate to get a nice clean extract.
The back-salting separates the alkaloids from the oils etc and enables a reduction of the solution to an easily managed amount. Uses less solvent and is cleaner.
Then proceed to boil phyllodes in solution that you mentioned however ethanol isnt neccessary now.
Instead of defatting you could just pull 4 times with 50-75ml of xylene (after base is added) then combine pulls.
Then back salt x5 with 50ml of vinegar.
Separate from xylene and put into a narrow bottle then basify with say 10g of lye or until pH 12-13. Add 100ml of salt saturated water.
Then pull x3 with 50ml of xylene and evaporate to get a nice clean extract.
The back-salting separates the alkaloids from the oils etc and enables a reduction of the solution to an easily managed amount. Uses less solvent and is cleaner.
Thanks for the info DReaMTripper.
Does the back salting allow for the extraction of all the other alkaloids present? I guess as long as you use xylene for the final pulls the broad spectrum alkaloids should still come into and across from the vinegar.
How would you go about doing a mini extraction on the first gum laden ethanol and water boil? Is it likely to have a significant yield? If I get nothing in the main extraction is it worth continuing onto the mini extraction?
Thanks again.
Does the back salting allow for the extraction of all the other alkaloids present? I guess as long as you use xylene for the final pulls the broad spectrum alkaloids should still come into and across from the vinegar.
How would you go about doing a mini extraction on the first gum laden ethanol and water boil? Is it likely to have a significant yield? If I get nothing in the main extraction is it worth continuing onto the mini extraction?
Thanks again.
DreaMTripper
Rising Star
- Merits
- 42
Its not likely to have much but you can extract by just filtering the liquid a few times then reduce, basify and pull with solvent.
Yes back salting with make all the alkaloids into salt form and migrate to the water.
Yes back salting with make all the alkaloids into salt form and migrate to the water.
Thanks --Shadow,
So here where I am methylated spirits is ethanol. So your saying soaking the phyllodes in ethanol with a few hot water baths and some shaking should get rid of the unwanted gums but leave the target alkaloids in the phyllodes. Then dry phyllodes and move onto the ethanol, water, vinegar boil (2/1/1). So no dmt will be lost in the initial ethanol soak?
If this is the case it sounds like an easier way to go given that a second mini extraction will not be required.
Thanks for your help guys.
So here where I am methylated spirits is ethanol. So your saying soaking the phyllodes in ethanol with a few hot water baths and some shaking should get rid of the unwanted gums but leave the target alkaloids in the phyllodes. Then dry phyllodes and move onto the ethanol, water, vinegar boil (2/1/1). So no dmt will be lost in the initial ethanol soak?
If this is the case it sounds like an easier way to go given that a second mini extraction will not be required.
Thanks for your help guys.
DreaMTripper
Rising Star
- Merits
- 42
When youre degumming with an alcohol be that ethanol or methylated spirits (95%ethanol/5%water in Aus) you will pull a small ammount of alkaloids with both the methods above.
If you are really bothered about doing a small extraction after then you can go with your first method minus the defat and back salt instead. But then you will have to filter multiple times and use more liquid as the gums will still be in the solution.
The hunch is some of the alks get trapped in the gums/tannins in solution and generally obstruct extraction.
You could keep them in but you would have to use more solution so they dont take up as much space.
If you are really bothered about doing a small extraction after then you can go with your first method minus the defat and back salt instead. But then you will have to filter multiple times and use more liquid as the gums will still be in the solution.
The hunch is some of the alks get trapped in the gums/tannins in solution and generally obstruct extraction.
You could keep them in but you would have to use more solution so they dont take up as much space.
- Merits
- 192
methylated spirits is NOT ethanol no matter where you`re from, its Methanol... Ethanol does not have a methyl group, methanol does, thats why its called `methylated` spirits.
And no, do NOT defat with ethanol nor methanol, they will most definitely pull your alkaloids. In fact, many people use either of those two solvents as a first step in an extraction, then evap the solvent, and proceed to further purify them.
And no, do NOT defat with ethanol nor methanol, they will most definitely pull your alkaloids. In fact, many people use either of those two solvents as a first step in an extraction, then evap the solvent, and proceed to further purify them.
DreaMTripper
Rising Star
- Merits
- 42
Check out the msds for diggers methylated spirits attached..
The above ethanol/metho wash idea was taken from here.. Acacia Extraction Workspace - A/B - Welcome to the DMT-Nexus see phyllode tek exp 3.. works well on acacia phyllodes.
If in doubt rahii maybe you would be comfortable following nens tek on the same page
The above ethanol/metho wash idea was taken from here.. Acacia Extraction Workspace - A/B - Welcome to the DMT-Nexus see phyllode tek exp 3.. works well on acacia phyllodes.
If in doubt rahii maybe you would be comfortable following nens tek on the same page
Thanks for the links DreaMTripper.
I have always assumed that because ethanol and methanol are polar/non polar solvents that mix into both polar and non polar solvents that they wouldn't be suitable for doing a/b extractions. Does anyone know if the ethanol locks some alkaloids in the undesired solvent, or does it just act as the desirable solvent?
I'm starting to lean towards doing a vinegar and water boil, 1 x defat with 100ml of xylene to pull the gum, basify, pull with 450ml of xylene, then back salt into vinegar, basify, pull with 450ml of xylene, evaporate.
I have found that when dealing with thick basified plant extract, you can quickly separate the nonpolar by placing into 2 jars and diluting with water to thin it out a bit.
I really hope there is some spice to pull.
Thanks for all your help folks.
I have always assumed that because ethanol and methanol are polar/non polar solvents that mix into both polar and non polar solvents that they wouldn't be suitable for doing a/b extractions. Does anyone know if the ethanol locks some alkaloids in the undesired solvent, or does it just act as the desirable solvent?
I'm starting to lean towards doing a vinegar and water boil, 1 x defat with 100ml of xylene to pull the gum, basify, pull with 450ml of xylene, then back salt into vinegar, basify, pull with 450ml of xylene, evaporate.
I have found that when dealing with thick basified plant extract, you can quickly separate the nonpolar by placing into 2 jars and diluting with water to thin it out a bit.
I really hope there is some spice to pull.
Thanks for all your help folks.
DreaMTripper
Rising Star
- Merits
- 42
Its a tried and tested old school method you will notice in that thread there was an extraction done using just methanol.
Something not to be considered by the kitchen chemist as its a dangerous highly volatile odourless solvent.
Like attracts like so especially going for a full spectrum unknown alkaloid profile there is no knowing what will stay in the ethanol/water solution.
In my opinion it is unneccessary to use ethanol on phyllodes after the gum/tannins etc have been stripped from the phyllodes surface other than to reduce quicker.
Nen sais it helps preserve the plants original alkaloid profile and that using prolonged heat may change that.
The reason for the ethanol/water boil is to strip away these brown gravy like (in solution) substances so the cells uderneath can be accessed for extraction. Bubbling hot ethanol and water does a great job of this in little time.
It will be interesting to see if xylene will be able to pull these gummy substances off the phyllodes just as effectively however there was one person who questioned whether xylene would also pull a small amount of alkaloid salts but this wasnt answered.
Your method described would work Im sure but you should definitely do a freeze-thaw beforehand to lyse the phyllodes.
Salt would also be a good thing to use its been proved effective in the max ion tek.
Once in the base stage the remaining gum seems to drop out of solution and causes a sediment that settles and like you said adding more water means it doesnt clog up the vessel.
450ml of xylene seems a great deal but if you have the patience and more importantly the ventillation then splitting up into small pulls will not leave many xylene soluble alkaloids left in. Good luck! Which plant is it?
Something not to be considered by the kitchen chemist as its a dangerous highly volatile odourless solvent.
Like attracts like so especially going for a full spectrum unknown alkaloid profile there is no knowing what will stay in the ethanol/water solution.
In my opinion it is unneccessary to use ethanol on phyllodes after the gum/tannins etc have been stripped from the phyllodes surface other than to reduce quicker.
Nen sais it helps preserve the plants original alkaloid profile and that using prolonged heat may change that.
The reason for the ethanol/water boil is to strip away these brown gravy like (in solution) substances so the cells uderneath can be accessed for extraction. Bubbling hot ethanol and water does a great job of this in little time.
It will be interesting to see if xylene will be able to pull these gummy substances off the phyllodes just as effectively however there was one person who questioned whether xylene would also pull a small amount of alkaloid salts but this wasnt answered.
Your method described would work Im sure but you should definitely do a freeze-thaw beforehand to lyse the phyllodes.
Salt would also be a good thing to use its been proved effective in the max ion tek.
Once in the base stage the remaining gum seems to drop out of solution and causes a sediment that settles and like you said adding more water means it doesnt clog up the vessel.
450ml of xylene seems a great deal but if you have the patience and more importantly the ventillation then splitting up into small pulls will not leave many xylene soluble alkaloids left in. Good luck! Which plant is it?
That has cleared a few things up. I am used to extracting Chacruna which doesn't have any gums to contend with so keep getting drawn away from trying to deal with this issue. The plant is A. Stigmat ophy...lla. This resinous shrub joins juliaflorae to plurinervens, both active subfamilies, so here is hoping. Given the small human population nearby to where this plant lives it is unlikely to ever be used much if active. I got my phyllodes from garden grown plants as the natural range is a long way from where I live.
I sort to clear up the issue of whether dmt acetate is soluble in xylene in this thread - Solubility of DMT acetate in Xylene - Advanced/Enhanced chemistry - Welcome to the DMT-Nexus
Seems it's not.
Think I might freeze thaw, keeping the water, then place phyllodes in a jar with vinegar and xylene, shaking well for a few days. This should pull the gums into the xylene but pull the alkaloids into the vinegar. Discard xylene, combine vinegar with melt water and boil phyllodes with excess water, continue with the base, salt, xylene, back salting with vinegar and basing out to xylene for evaporation.
I'll leave it at that for now, it's a lot of information to work with. If there are actives in the phyllodes I'm sure to pull something.
I'll let you know how I go. Could be some time before I can undertake the tek but I will report back after.
Thanks again for your help folks.
I sort to clear up the issue of whether dmt acetate is soluble in xylene in this thread - Solubility of DMT acetate in Xylene - Advanced/Enhanced chemistry - Welcome to the DMT-Nexus
Seems it's not.
Think I might freeze thaw, keeping the water, then place phyllodes in a jar with vinegar and xylene, shaking well for a few days. This should pull the gums into the xylene but pull the alkaloids into the vinegar. Discard xylene, combine vinegar with melt water and boil phyllodes with excess water, continue with the base, salt, xylene, back salting with vinegar and basing out to xylene for evaporation.
I'll leave it at that for now, it's a lot of information to work with. If there are actives in the phyllodes I'm sure to pull something.
I'll let you know how I go. Could be some time before I can undertake the tek but I will report back after.
Thanks again for your help folks.
DreaMTripper
Rising Star
- Merits
- 42
Will keep my fingers crossed for you if you get a sufficient yeild condider sending some for analysis.
I have read some old comments today that despite the MSDS of reochems diggers methylated spirits stating only 95/5 ethanol/water it does have other undesirable chemicals in it. So avoid. Like the plague.
I have read some old comments today that despite the MSDS of reochems diggers methylated spirits stating only 95/5 ethanol/water it does have other undesirable chemicals in it. So avoid. Like the plague.
Hieronymous
Rising Star
- Merits
- 42
Thanks for the update Rahli
Just out of curiosity how did the xylene de-fat go ?
Did you see much crap in the de-fat solvent and did the final evap leave any residue or just an empty dish ?
Just out of curiosity how did the xylene de-fat go ?
Did you see much crap in the de-fat solvent and did the final evap leave any residue or just an empty dish ?
DreaMTripper
Rising Star
- Merits
- 42
Shame, good on you for trying thanks for updating.
I think the tek worked well as far as I could tell without being able to pull some yield.
The xylene took a few days in the jar to start pulling all the resins out of the phyllodes but it was fine after around 4 days. Mixing in some vinegar should pull any spice that is extracted in the xylene.
First I did the freeze defrost and got a fair bit of resin in that too. i have decided not to do an extraction on that as I got nothing in the second part of the tek so it is highly likely devoid and I don't wish to waste any more effort on poor material when I have plenty of good quality alternative.
I did pull a tiny speck of extract but it doesn't smell of anything so I doubt it is active. even if it is active I wouldn't waste my time again extracting a speck of material.
The xylene took a few days in the jar to start pulling all the resins out of the phyllodes but it was fine after around 4 days. Mixing in some vinegar should pull any spice that is extracted in the xylene.
First I did the freeze defrost and got a fair bit of resin in that too. i have decided not to do an extraction on that as I got nothing in the second part of the tek so it is highly likely devoid and I don't wish to waste any more effort on poor material when I have plenty of good quality alternative.
I did pull a tiny speck of extract but it doesn't smell of anything so I doubt it is active. even if it is active I wouldn't waste my time again extracting a speck of material.
