Extraction method without solvent

[Explorer2023]

This is a method of extraction without using solvents which I have done in the past.
It was experimental on unknown plant acacia species.

In essence it is simply an acid/base cycle and clean with demineralised water flushes.
It takes a lot of time but yields alkaloids.

Step 1) grind plant bark or leaves in garden mulcher.

Step 2) place in crock pot and boil with water and vineger, outside on a on gas camping stove, for about 1-2 hours. Let it cool to around room temperature.

Step 3) Pour liquid into a glass jug, filtering through a cloth fabric, and let stand for 4-6 hours for fine particulates to accumulate on bottom.

Step 4) With a plastic tube siphon the liquid into second glass jug careful not to suck up the debris from the bottom. discard the debris.
(Optional repeat stage 2 and 3).

Step 5) Now prepare an alkaline solution by premixing sodium hydroxide (NaOH) into demineralised water (adding the NaOH to the water, not the other way round).

Step 6) Slowly add the alkaline solution to the acidic water extraction, small amounts at a time and stir. Slowly the water will turn black and alkaloids will begin to precipitate from the liquid.

Step 7) Let it sit for 12 -24 hours for precipitation to collect at bottom of glass jug.

Step 8 ) With a plastic tube siphon of the liquid, this time leaving the precipitation at the bottom. Discard the liquid.

Step 9) Do 2-3 washes on the precipitate with about 100 ml of demineralised water to wash out the NaOH. Because the particles are freebase they will not redisolve into water. Add about 100 ml of demineralised water to the collected freebase alkaloids and gently swish it around. (Optional transfer into small glass jar). Repeat step 7 and 8. Do this two or three times.

Stage 10) place extraction on shallow dish and let the excess water evaporate. You'll have clean dry freebase alkaloids (powder).

 

[Brennendes Wasser]

When adding the NaOH actually you will get voluminous white clouds of (probably) DMT just at pH 7,5+. I always thought what will happen if I would just try to collect those, but they are probably too fine to ever be filtered. Then if adding more base as you tell it will go dark - while the clouds will also vanish. So I thought DMT will for some weird reason dissolve again at pH > 10.

But that means you can still get some precipitation? Could be a nice thing, as you would not get any risk for emulsions. How does the final product look like - is it very fine dust and therefore you might spill some over, when decanting water?

And probably biggest question what is the yield?

 

[Explorer2023]

When adding the NaOH actually you will get voluminous white clouds of (probably) DMT just at pH 7,5+. I always thought what will happen if I would just try to collect those, but they are probably too fine to ever be filtered. Then if adding more base as you tell it will go dark - while the clouds will also vanish. So I thought DMT will for some weird reason dissolve again at pH > 10.

But that means you can still get some precipitation? Could be a nice thing, as you would not get any risk for emulsions. How does the final product look like - is it very fine dust and therefore you might spill some over, when decanting water?

And probably biggest question what is the yield?

Ah true that is interesting. Just let gravity do the work. With a PH of 7.5 the precipitation may stay suspended for longer but will eventually fall to the bottom. It helps to use a a tall and narrow jug with vertical walls as opposed to a dish with a wide base area. Some percipitation may also stick the sides, a gentle tap with a solid rod every few hours helps unstick them. Suppose with a neutral PH it would'nt exactly need the 3x water flushes, perhaps just one for good measure.

It is a very fine dust. Have to be carefull not to lose the precipitation while decanting. can expect to lose some but if done correctly can keep it minimum. Siphoning with plastic tube is better as it doesn't agitate the solution.

The yield is a fine dry powder, because I was experimenting with unknown species it's also unknown composition. Ofcouse from that stage can do many thing such as for example convert back into an acid and redisolve in anhydrous acetone.

 

[ShadedSelf]

Seems like the OP deleted their post?

I decided to give it a go with some Acacia Confusa sample that I had lying around.
After adding NaOH it went dark even before reaching a ph of 10.
Id say the solution gets a bit cloudier, bit its hard to tell, either way it all seems to stay in suspension.

Out of dissapointment I tried adding some NaCl just to see if something could happen, and now there is definitely "stuff" precipitating, I tried adding salt to the acidid solution but that doesnt seem create any sort of precipitation.

I guess now I have to find out wether this stuff is DMT or not.