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MHRB Soxhlet Extraction

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D_Juggz

D_Juggz

Dr Do Little
Hey peoples, I thought that I should get the ball rolling. There are a few of us nexians who are interested in soxhlet extraction, I will gather Ideas here for MHRB extraction and then hopefully condense this thread into a workable Tek.
So far this is my hypothesis:
:arrow: :arrow: :arrow: :arrow: :arrow:
Need:
*Soxhlet
*Condenser
*Water pump
*Water bucket
*Tubing
*MHRB
*Naptha
*IPA

Procedure:
1. Set up soxhlet - make sure its connected to cool water supply before put on heat
2. Fill Soxhlet body with MHRB, Cotton ball at bottom and top.
3. Add 9% Vinegar (To the soxhlet body) compared to the total amount of IPA that will be added, let it sit there for an hour (should be ~pH=3)
4. Fill with IPA 99% (A good amount is when it clears itself x3) --will depend on the size of soxhlet
5. Put the soxhlet on heat, and boil solvent for ~8-12 hours (do not let the solvent get too thick, or it could burn off the alkaloids.)
6. Once finished you will be left with DMT acetate in an IPA/water solution.
7. May need to do a naptha defat if product looks oily. --this process still needs to be described.

Defat Step
Starting with the acidic IPA/Water/Dmt acetate solution
1. add hot naptha to solution and gently swirl for 5mins
2. decant or separate the naptha off
3. repeat step 1 & 2
4. repeat step 1 & 2
5. add more naptha, then basify and mix well
6. separate naptha & do freeze percip.



Questions:
1.
2.
3.

Hints:
Soxhlet extraction is the fastest when the highest heat on the hotplate is used. So it’s always best if the condenser is operating well at the highest heat used. If not, switching to a larger condenser is always better than turning down the heat because its faster. But when using a low boiling point solvent like DCM, you often need to turn down the heat, even when using a very large condenser.

Make sure you put stop cock grease on all the glass joints (or Teflon tape, or Teflon sleeves) before connecting the glass ware. If you don’t, the glass pieces can get stuck together permanently. SWIM prefers Teflon joint sleeves, but these cost a lot. Teflon tape (the kind used for plumbing) is really cheap and works really well. Just wrap the joints a few times with Teflon tape and then connect them. It makes a water tight seal and prevents the glass joints from sticking together. SWIM doesn’t like stop cock grease. It’s messy and sticky. And if using DCM, it will dissolve into the DCM.

Also make sure to clamp everything to a good sized lab stand so that nothing falls over and breaks. Soxhlets are pricey. The last thing you want is it accidentally falling over.

You can keep adding new plant material over and over and over if you like. Normally 8 hours is sufficient to get about 99% of all the desired compounds out. This varies depending on the plant material and whether it’s whole pieces (could take 10-12 hours) or coarsely ground material (could take 4-6 hours). You can tell usually by the color of the solvent in the bottom of the Soxhlet. As the Soxhlet runs, the solvent in the Soxhlet gets lighter and lighter colored as the solvent in the boiling flask below it gets darker. Once about 99% is extracted, the liquid in the Soxhlet looks clear with a very slight yellow hue. At that point you can discard the used plant matter and put fresh plant matter in it. Just don’t let the liquid in the boiling flask get thick. As long as it’s watery and not thick, you can keep going and going.

Thanks to Ron for all your help! (back in the day)
 
What are you filling with the acetic acid and allowing to sit for an hour? Is this the biomass outside of the apparatus (prior to extraction) or inside the apparatus?

I would start with a very simple non-polar extraction with something like Naptha/DCM and extract all that I can from the plant mass. Then i would distill off the solvent (for recycling and to expose my organic extracts), leaving a yellow goo/oil/crystal mix in my flask... THEN i would utilize an A/B on this extracted aggregate of goodies for the desired compounds.

In theory, you should be able to add some DH20 acidified to pH3 (pure/distilled water), this would pop your [desired] compounds into the water and leave your oils to be extracted with a your solvent. Do the solvent wash and decant the solvant (and oils).

Add more clean solvent and bring your water pH back up (pH 12-ish) which should pop your [desired] compounds back into the solvent where you can decant off and evap/freeze precip etc. for a pretty clean end product.

This is all theory of course.. but with few variables, and known processes. Starting off a warm extraction with IPA and 30% acetic acid sounds like difficulty ahead to me... but im no chemist nor do I claim to be.. thats just a lot of water.

If Im way off here I'm sure some of the resident experts will help me out (kindly I do hope :oops: )
 
Putting the acetic acid + plant matter within the soxhlet (easier than doing it ouside and then transferring.)
Letting it rest in acid will make sure that more DMT is pulled faster. Theoretically) -- Although the DMT is already in water/IPA soluble salt form within the MHRB so it shouldn't make a huge difference if you skip this step.

This thread isn't really to debate whether soxhlets are easier or whatever...there is another thread for that. the whole point here is to use the soxhlet for extraction.

You are right though - i got the 30% from 69Ron (it does sound like a lot and might slow it down), but i have found 91%:9% (IPA:Water/Vinegar) works well... will test it soon to see which works best.
 
There was no intention to debate the value of soxhlet extraction. I apologize if my post came off that way.

I was under the impression that it was an open thread for an accumulation of ideas and experiences pertaining to the development of a soxhlet tek, and there fore I was just indicating one possible route.

Another thought about the acetic acid... I wonder if one could do the initial extraction with just acetic acid, effectively doing warm acid wash like the many crock-pot teks. Then simply basify the acetic acid solution and do non-polar wash to pull off the goodies? .. Humm.. might have to break out some glass, dust it off and put some effort into helping this thread along.
 
Your right, i didn't see the sox part, cheers.
You could definitely only use vinegar in the sox as the solvent, It would be much slower though (SWIM has tried) I suspect its because water doesn't boil as readily as IPA.
SWIM has never used MHRB though so he wouldn't know how much oil will actually be present, from what I remember reading there isn't that much.
Would have considered DCM, but there doesn't seem to be many pure stuff commonly available (maybe thats just here)
Maybe I was wrong about IPA 91% being miscible in naptha...will go test it and post back.
 
Anybody experimented with IPA diluted to different concentration, like 40%, 60%, 80%? Why exactly 91%?

Did anybody tried phosphoric acid instead of vinegar? It seeems to work exceptionally well for aya.
 
So it would be reasonable to say, that one could (once all the spice has been extracted with the soxhlet) boil off the IPA and add more water (which is not miscible in naptha)
Then, you could add naptha & basify pulling the spice into the naptha.
Then you could defat from there and then crystallize or salt into DMT fumarate.
 
D_Juggz said:
So it would be reasonable to say, that one could (once all the spice has been extracted with the soxhlet) boil off the IPA and add more water (which is not miscible in naptha)
Then, you could add naptha & basify pulling the spice into the naptha.
Then you could defat from there and then crystallize or salt into DMT fumarate.
Click to expand...

SWIM defats with heptane BEFORE basifying.
 
but if you dont basify, then the dmt wont move into the solvent...right?
any particular reason for using heptane? i dont think its as easy to find as naptha.
 
D_Juggz said:
but if you dont basify, then the dmt wont move into the solvent...right?
any particular reason for using heptane? i dont think its as easy to find as naptha.
Click to expand...

You pull spice with naphta after basifying because it is in FB form therefore soluble in non-polar solvents like naphta. If you defat basic solution a lot of spice will be lost.

When the extraction is in acidic water/IPA solution then spice is in the form of appropriate salt and not soluble in naphta. So defatting the acidic solution will not lead to spice losses.

This is SWIM's theory though she is not a chemist.

SWIM does not use naphta because she has access to lab grade heptane.
 
Benzyme, i realize this is another topic all together, but for the sake of having very pure product, SWIM would like to do a defat.
Could you perhaps explain how to proceed with chemicals available to non-lab people? - how much product would be lost in the process?
Also, do you see any flaws in my reasoning in the above tek?
 
I am kind of clueless as how to proceed after extracting for 12 hours in a soxhlet and boiling the solvent to get a low volume solution.
Please advise.. with some approximate quantities of substances to be used too. thanks
 
Well, you could just take the condenser off the soxhlet and boil it down to a manageable amount.
The solvent should evap first, leaving behind DMT acetate in water basically...but I'm not sure if boiling on a high heat is a good idea...maybe it is...any advice here?
SWIM would boil the IPA off at a mid heat (just enough to start a slight boil) - shouldn't take too long.
Alternatively, use a smaller soxhlet with less solvent.
 
if one already has a soxhlet, one should also consider getting a pressure-equalizing dropping (addition) funnel to place between the extractor body and the condenser. with this setup, one may recover the solvent for later use.

benzyme said:
to recover clean solvent, it would be more effective to use a pressure-equalizing dropping funnel between the extractor body and condenser.

it looks like this
9c_1_b.JPG


you keep the valve open during the extraction, and close it when you're done extracting and want to reduce the volume in the rbf, to recover your solvent.
Click to expand...
 
You can recover the solvent by just removing the plant mass and cleaning the extractor, after the soxhlet refluxes one last time. then you start it again and the solvent will be in the extractor body, which can be poured without much difficulty using a funnel.

D_Juggz: so you're telling me a soxhlet extraction with IPA, vinegar (water+ acetic acid) only pulls out dmt acetate from mimosa? come on. My extract is a black goo, that needs to be further purified.. already been reduced to a workable ammount. So what is the next step?
 
There is more than just dmt acetate and water at this point.
Next step would be a defat with naptha.

This would be your typical A/B but replacing the 3 boils with a more efficient way of removing alks from the plant matter. So at this point it's the normal A/B steps.
 
ok, can you elaborate on these a/b steps, given the initial extraction method with vinegar/ipa? just to make sure, i don't want to lose or make my crystals too complicated to get by doing the wrong thing :(
 
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