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Salt-free harmala extraction? Options
 
blue.magic
#1 Posted : 4/3/2018 10:30:22 PM

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I was thinking about rue extraction that does not require immense amounts of salt and came up with the following process.

Do you think this might work?

- extract in water (e.g. boil, filter, combine water extracts)
- filter
- boil off excess water
- filter
- base with Na2CO3, NaOH or KOH
- wash with water, decant supernatant liquid, add fresh water, repeat few times
- filter, scrape alkaloid extract
- dissolve freebase harmalas in dilute HCl or vinegar
- filter
( repeat basing and salting for extra purity)
- dissolve freebase harmalas in small amount of dilute HCl
- dry

The only issue I see with this may be that some toxic alkaloids may get too concentrated. These are stripped off by Manske step in the traditional tek.

An interesting experiment might be to crystallize this harmala HCl extract and boil off the filtrate, then calculate weight of the residue minus the weight of salt used. This will give the total weight of impurities. Then we can compare this to the traditional tek.
 

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ShamensStamen
#2 Posted : 4/4/2018 1:11:54 AM
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That's pretty much what i do, but i stick to freebased extracts, you only need HCL extract or Harmalas in salt form if you wanna separate it from other alkaloids in the full spectrum extract (which there's nothing really wrong with those other alkaloids ime).

I just boil up 100 grams of whole Rue seed, do about 4 to 6 separate boils straining/filtering each boil off into a big pot, reduce the boils and boil it all down to about 375 to 400mls, add in 75mls of vinegar, dissolve like 15 to 20 grams of washing soda into 100mls of hot water, pour/stir the washing soda water into the brew which precipitates out the crude full spectrum extract.

Once the extract falls to the bottom over say 30 minutes or so, i pour off the top water through a coffee filter (just in case) and continue pouring the extract into the filter, i rinse the measuring cup with fresh water to make sure i get all the extract out and into the filter, once all the liquid is drained through and the extract is in the filter, i dunk the open filter into about 300 to 400mls of fresh warm water with 75mls of vinegar added and make sure all the extract falls off the filter into the water and stir until it's dissolved (i also wet the filter a little bit with some extra fresh water and wring it out in the measuring cup a few times to make sure i get everything), once it's all dissolved it's filtered, re-based and filtered again, i re-dissolve, filter, re-base, and filter a couple more times or so until i have a pure full spectrum freebased Rue extract.

Once it's clean i twist up the coffee filter with the extract in it, getting out any air or moisture, put it into a paper towel and press on it to compact it but also to squeeze out any excess moisture, and then i open back up the coffee filter and let it sit out to dry, and while drying i break up the extract clumps in order to let it more fully dry. Once dry i put it into a container and can either smoke some or encapsulate some and take it orally, or dissolve it in something acidic if i want to drink it.

But with that said, i don't think simply drying an acidic extract liquid would give you a good powder, probably more of a residue, but for an actual Harmala powder, you need to do a manske extract on it which just requires 100 grams or so of salt if i remember correctly. Some people do their manskes multiple times but i've only ever done it one time and i've done the manske extraction a few times, seemed pure enough to me and was certainly different compared to the full spectrum freebased extract so i'm pretty sure one salting was enough to leave behind most of the other alkaloids.
 
Elrik
#3 Posted : 4/4/2018 3:37:35 AM

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I tried this before. All the precipitated plant gunk in my try made it muddy, difficult to settle, and impossible to filter.
I probably had it fairly concentrated, as I was processing 3/4 of a kilo. That may have been a major factor. In the end I added vinegar and salted the goodies out Laughing

Watch the gunk.
 
blue.magic
#4 Posted : 4/4/2018 4:46:22 AM

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Okay so here are the results. It worked out perfectly!

I simply added the FB powder in a small amount of water and mixed in twice the stoichometric amount of HCl (approx. 2 ml of 3.5% HCl to 300 mg harmine).

I poured the solution in a Pyrex dish and evaporated. The scraped material is not completely dried since I was in hurry to post the results, but I it will powderize easily after further drying. It's not gunky at all, just nice golden hairy harmala xtals Pleased

I am a little suspicious the FB material was Mansked at least once so I cannot confirm this will work for "salt-free rue extraction". I will try going from seeds and post the results. I sometimes process 100s of grams of rue seeds at once and the promise of not needing to purchase kilos of salt is pleasant.

...under LED light:


...under fluorescent light tube:


scraped xtals:


300 mg harmine freebase in a small amount of water:


fully reacted with HCl - some tiny impurities occured, now it's opportunity to filter if needed:


harmine.HCl solution dumped in Pyrex:


fluorescent xtals happily growing:
 
blue.magic
#5 Posted : 4/4/2018 4:58:49 AM

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Elrik wrote:
I tried this before. All the precipitated plant gunk in my try made it muddy, difficult to settle, and impossible to filter.
I probably had it fairly concentrated, as I was processing 3/4 of a kilo. That may have been a major factor. In the end I added vinegar and salted the goodies out Laughing

Watch the gunk.


This happened to me but with yellow caapi. The stuff simply stayed suspended in the solution and it took whole night for it to at least partially settle. It was possible to filter but I lost quite a lot of product in the process.

With 500g rue, I do 1200 ml acidic soak, then 3x 1500 ml 30 min boils, let the the combined water extractions settle (few hours suffice), vacuum filter through loose cotton, reduce to 1200 ml, filter through loose cotton, tight cotton, paper, base with NaOH, filter with paper, dissolve in hot vinegar, filter, (repeat twice), last filtering is through a bed of diatomaceous earth and the last basing is with Na2CO3.
 
blue.magic
#6 Posted : 4/9/2018 8:41:25 AM

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Okay I have tried to produce harmala hydrochlorides directly (without Manske). Of course, the resulting powder is hard to scrape and very dirty (all the impurities are perfectly water-soluble though). Still somewhat crystalline.

I will later try to crystalize harmalas using just HCl and 10% saline to see if the absence of vinegar makes any difference.

The final step of mixing freebase harmalas with dilute HCl and evaporating allows one to get without any vinegar or salt contamination since the freebase can be thoroughly wased with water.
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