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No-boil acid soak for cleaner extractions

Stochastic

Esteemed member
I'm interested in compiling experiences of no-heat acid base extractions, especially of ACRB. I always had success with MHRB but after several failed attempts over the years with wild-harvested ACRB I wanted to try something different.

An acid boil (with or without added acid, as the water will acidify from the rootbark alone) will extract tannins and other substances, including lipophilic compounds. ACRB is composed of about 28% extractable condensed tannins and 19% other phenolics.

DMT has a MW of 188. The tannins have MW of about 1000-3300.
They're also generally more tightly bound in the structure of the bark than the DMT.
Tannins stabilize emulsions and would be best to minimize in the extraction process.

So, all that said, a room-temperature acid soak seems to be the cleanest route to an extraction, as the following posts attest.

My question is: does anyone have any experience around the effects of soak time, volume, and pH on yield? One poster recommended soaking for several weeks; another got high yields after soaking overnight, decanting, refrigerating to remove waxy deposit, and basifying.

...


Soak MHRB in vinegar for a couple weeks, or a month if you like. Don't heat it. Heating only causes problems in filtration and doesn't improve the extraction any further. After a room temp vinegar soak, filtration is very easy and be done in 5 minutes. I like to use a nylon nutmilk bag. Seems like a single soak like this can extract 85-90% of the alkaloids, maybe more.
It makes life easier during the extraction because you don't have to deal with STB sludge, so it speeds up the liquid-liquid extraction process significantly.


I soaked 85g of ACRB in cold vinegar 3 times. It came out very clear. I filtered it and reduced it to 90ml. I let it settle in the fridge and decanted, leaving behind an oily, water-insoluble sediment. This cleared it up even more. It was, however, still astringent.

I transferred it to a 200ml jar, added some salt and based it with lye to pH 12.3. It clouded with tiny crystals, which was reminiscent of the harmala basing of the acidic soup in rue extractions.
My first thought was "Is this DMT?"

I added ~90ml of naphtha and after some mixing, much of the crystals floated to the top (DMT being attracted to naphtha?) forming a layer between the water and naphtha, some sank to the bottom, and a lot of them stayed in suspension, which I didn't wait to let settle.

After each pull, there was less and less of the visible crystals in the aqueous layer.

I backsalted the pulls with vinegar and the first pull was so rich in DMT, it precipitated on the walls of the glass within a couple of minutes. Not as pretty crystals though, but rather small white blobs.

Summary:

1. Cold soaks are much cleaner than boils, making for cleaner extractions.

2. The extractions are so clean that the volume can be reduced significantly (100 ml per 100 g of bark, or even more concentrated) without affecting the extraction. No risk of emulsions (with naphtha anyway), and it's much easier to handle the smaller jars.

3. Now, this needs to be tested further, but an NP solvent may not even be necessary; instead, a rue-style extraction may be performed, whereby the acidic cold soaks are based, then allowed to settle, decanted and filtered - and this may work especially well with smaller water volumes. If this is not clean enough for a desired end product, this may be processed further (mini A/B, re-X etc.). For oral, however, after dissolving in vinegar or similar acid this precipitate may be clean enough.

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my bark was shredded. I did 3 soaks, the first one 'as is', the 2nd one following a freeze-thaw cycle, and the 3rd one following another freeze-thaw cycle and further shredding in a Nutribullet, which just produced finer pieces, but nothing close to a powder.

Now, I don't know whether that was needed; some of it may have been redundant. According to Mindlusion, just one cold soak, with enough liquid to cover the bark, should remove ~85% of the DMT.
He suggested a long soak, in the order of a month; mine, on the other hand, were short: the 1st one was overnight, the 2nd and 3rd were no more than a couple of days.


After a few 75 g extractions went further south than i planned, couple emulsions, a poor yield, I've been able to replicate the same yield with the same consistency three times.

I think the trick has been 100mls vinegar added to the bark in 400 mils water and letting that sit in front of my space heater in my room for 12 to 24 hours.

...

a rounded down 2g from 75g bark gives a over 2% yield
 
Well, I got very rapid precipitation of pure white crystals; the naphtha (ronsonol lighter fluid) was clear again within a few hours. I poured out the naphtha, turned the jar over, and put it back in the freezer for several more hours. Then I put the jar before a fan to dry.

The result was a clear white goo which is extremely acrid when tasted, definitely can't be smoked. This has happened every other time I've tried to extract ACRB I harvested in Hawaii, whether STB or A/B, defat or no, and now no-boil. There's no chance of contamination by the aqueous phase, I was meticulous and the result was completely white.

Any insights?
 
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