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Does DMT precipitates as tannate in MHRB mother liquor? Options
 
blue.magic
#1 Posted : 10/22/2019 12:44:57 AM

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I am a fan of A/B extraction path, but recently I became suspicious that DMT might get lost in my process by filtration.

I usually filter everything with cheesecloth and cotton wool, and the wash the residual sludge by mixing with hot fresh water, letting cool down and re-filter.

However, if DMT exists as tannate even in mother liquor containing generous amount of acetic acid (50 mL/L), I am afraid it might precipitate with other tannins and never get through the filtration process.

My preparation process looks like this:

- boil shredded+ground MHRB 4x in acidified water (small amount of acetic acid added)
- strain each boil to a large pot through moderately fine sieve (about 1 mm mesh)
- let the pot with combined liquid sit overnight
- decant supernatant, cover the sludge with twice its volume of hot water and mix
- let the sludgey water sit until cold, then decant and press the sludge through a cheesecloth
- reduce all the liquid
- let the concentrate sit overnight
- filter the concentrate through the cheesecloth, press the fine sludge as much as possible
- re-filter through cotton wool
- basify, extract etc.

I wonder how many alkaloids is trapped in the sludge, but the tannates might explain why I get yields of 0.4-0.6% instead of 0.8-1.0% more typical to the high quality MHRB inner root bark.

I like A/B teks over STB as I like to use as little base as possible, protect my glassware from strong bases, be able to use separatory funnel and finally to avoid emulsions caused by small particulates (I believe filtering the basic soup is hard and dangerous).
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Jagube
#2 Posted : 10/22/2019 10:14:10 AM

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I don't know, but if that's the case, maybe a stronger acid would displace the tannate ion? Have you tried brewing with phosphoric acid?

I think the yield for MHRB extractions should be closer to 3%, at least with Cyb's Max Ion tek. I've only ever extracted from MHRB once, as my first ever extraction, and got 1.5% with naphtha freeze precipitation, without solvent evaporation, then pulled with sunflower oil and got what I think was equivalent to another 0.3%. So all in all, close to 2%. And that was with MHRB brewed with vinegar.
 
endlessness
#3 Posted : 10/22/2019 10:26:19 AM

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Dont filter after reducing, filter before reducing only. There are papers talking about ayahuasca sludge containing alkaloids. In concentrated solutions its not unreasonable to imagine DMT tannate precipitates.


Mimosa yield is usually around 1-2%, I don't think 3% is common at all.
 
Jagube
#4 Posted : 10/22/2019 10:33:57 AM

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endlessness wrote:
Dont filter after reducing, filter before only. There are papers talking about ayahuasca sludge containing alkaloids.

For tea (as opposed to extractions), I like to also filter after reducing, as I don't want to have solids in my tea. But instead of discarding the solids, I put them in a pan, add water and a dash of vinegar, and 'brew' them. This pulls a lot of actives into the water, which I add to the first filtrate. As a result, I still end up with a clean tea, free from solids, yet the yield is still high, probably an extra 25% compared to if I discarded the solids.

The brewing of the dregs is quick, something like 2 boils with little water 5 minutes each does the trick.
 
endlessness
#5 Posted : 10/22/2019 10:40:05 AM

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Indeed that's a good strategy.
 
coAsTal
#6 Posted : 10/22/2019 4:33:08 PM

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You could just as easily perform the egg white tek to bind all the tannins and clarify your brew.

I have used that method for years to clean up caapi prior to my final reduction.


Here's where this thread interests me-- I have seriously considered lately eating the egg white, to see if the tannins, bound to the egg protein, would not cause the nausea that the tannins do in solution-- it would also possibly make metabolization of the alks easier.

Do you guys have any thoughts on that? It may just be a crazy assumption... but FWIW the egg glows brightly flourescent under UV post-tannin/solids extraction... so I know there's some alks in there... (although I've never had an unexpected reduction in trip quality after, so I know most of the alks are retained in the liquid remaining)

If blue.magic is right, the tannate alks would simply bind to the egg, which would be available via ingestion.

 
doubledog
#7 Posted : 10/22/2019 6:33:48 PM

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I know very little about chemical background, but know that every method of cleansing, fine filtering, decanting from sludge, using coagulant agents like eggwhites somehow decrease potency of the brew.

There are definitely some alks binded to eggwhites.
 
coAsTal
#8 Posted : 10/22/2019 7:50:09 PM

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The question I have is whether or not the eaten egg white would make a difference in the stomach discomfort that tannins cause-- as I wrote in the post above, there's no doubt that some alks are captured by the liquid eggwhite (and as you mention, any other filtration method to some variable degree), but it has not ever lessened the expected effects of a measured amount of caapi in my experience-- I have in the past used the egg-binding method and simple physical sediment filtering from the same supply with no felt strength differences.

So while there are some alks lost, I believe them to be relatively minor-- but if I could reclaim those minor losses in a semi-palatable way that didn't induce purge (I rarely ever do) I would be interested.

I guess will find out for myself next time I brew aya, I think, though that may be some time... it was an aya-heavy summer, and I'm out of phase with it cold outside...
 
doubledog
#9 Posted : 10/22/2019 9:09:17 PM

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My guess is that eggwhites combined with dmt tannins will induce more stomach discomfort.
 
blue.magic
#10 Posted : 10/30/2019 1:45:26 AM

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endlessness wrote:
Dont filter after reducing, filter before reducing only. There are papers talking about ayahuasca sludge containing alkaloids. In concentrated solutions its not unreasonable to imagine DMT tannate precipitates.


Mimosa yield is usually around 1-2%, I don't think 3% is common at all.


The problem is that if I dont't filter the reduced tea, it clogs my sep. funnel.

The fine particulates in the tea also turn into a kind of sludge after adding base, which seems to trap the solvent.

Sometimes I get a horrible emulsion which I believe is caused by the fine particles.

Here is the emulsion after extraction, it does not go away even after 2 weeks. Any stirring or heating makes it worse, a kind of "whipped cream":



Here is the closeup, the large bubbles have hard time to break:



I found that after adding copious amounts of drying agent (magnesium sulfate) and filtering the heptane/water/oil/sludge, there a brown oily layer:



I originally thought the brown stuff this is aqueous layer, but it behaves like oil and my indicator solutoion (nitrazine yellow) does not dissolve in it nor colorize it, rather breaks into small water bubbles.

I tried mini-A/B and without using that oily part and everything went well, but I think I will lose a lot of product in the oily layer. When I add the brown oily part to the sep. funnel, it fuses with the aqueous layer and forms emultions at high-pH:



It's like some kind of emulsifier. When I acidify the system, there is no emulsion, everything clears up in 2-layers quickly. However, when I continue adding base, the aqueous layer clouds up, thickens and finally merges with the heptane layer.

I am lost. This happens only sometimes, my guess is that my mother liquor is too concentrated and there are too much plant oils that saponify.

I am now seriously thinking about de-fatting or basify->re-acidify->re-filter like I do with harmalas.

Another option might be to get the liquour less concentrated (I use 4 mL water per gram of MHRB).
 
endlessness
#11 Posted : 10/30/2019 10:27:08 AM

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I'd def dilute the whole thing at least a bit.

Also you can consider filtering the sludge after reducing but then running hot water on the sludge that was filtered, to recover alkaloids there.

Another thing you can do is instead of using a separatory funnel at first, using a pipette or similar to suck up the top layer. I know it seems like a regression once you have used separatory funnel before but I think you can first do the pipetting with a large pipette and not being too careful, so that even if a little base layer comes through, you just add that solvent+maybe little bit of basified liquid in the separatory funnel, and use the opportunity to wash it with some sodium carb water. That way it will only be a bit you're draining at the bottom, won't be clogging your sep funnel.

For resolving emulsions I wouldn't stir nor use heat, I preffer putting on top of washing machine or loudspeakers or any source of constant mild vibration. Also using tons of table salt works.
 
blue.magic
#12 Posted : 10/30/2019 11:23:49 AM

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Okay I will try these steps in the next run.

As for the mini-A/B fail, it was my bad since I decided to recover a whole lot of old oily DMT without calculating the expected amount and perhaps made the aqueous solution too concentrated (I use 5-10% acetic acid for salting DMT).

No problem with pipetting Smile Whatever works best...
 
tripwire
#13 Posted : 6/7/2020 4:44:55 PM
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Its the reducing that makes the tannins precipitate taking the alkaloids with it. It is barely possible to reduce combined washes by even 50% without making the tannins start to drop. For this reason alone I find it impractical to embark on any of the boil, collect, boil, collect, filter, reduce, filter strategies to try to work with nice clean solutions.

The way round it is to go STB in large containers containing all the plant material. Make the dirty pulls with limonene. Then multiple back-salt into vinegar which can be combined, reduced filtered.

Now you have the starting point you want except you have gained better yield, haven't had to strain all that material, and haven't had to do large scale reducing of acidic solutions.
 
 
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