Harmalas Extraction and Separation Guide

[ava69]

Post #12 with pics of how to easily separate harmine and harmaline out with precision purity using drops of 10% janitorial strength ammonium hydroxide from hardware store and convert harmaline (RIMA) to the psychedelic or entheogenic pure tetrahydroharmine or THH (SRI) in only 1.5 hour, long time chemist, this is easy to do:

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[Phenethylamine23]

Sorry to be a pain. But wouldn't step 9 of the original method be filtering out crashed out alkaloids? If the tea extract is filtered thoroughly before reducing, the only thing crashing out of the solution would be the water soluble alkaloids as the water evaporates. You could be loosing precious alkaloids and for what? Mistakenly thinking it is plant material.

In actual fact step 3, 6 and 7 are filter steps to seperate non soluble plant matter, and still in step 9 have to filter again. This tells me the filtration steps are inefficient and could be improved.

I find the best way to filter plant particles is by letting gravity do it's work. Simply let the tea sit for a number of hours for sediment to form on the bottom then siphon out the liquid.

Also what was the yield from the 200g starting seeed weight?

 

[doubledog]

I would suggest to not filter rue tea at all, such step is not needed and is very annoying.
You can directly base tea still with some sediment in it if you want, it does not matter much.
First filtering is necessary only after dissolving precipitated freebase again in acidic water.

I agree that sedimentation/decanting method is great and should be preffered over filtering.

But it's common in plant extractions that after concentration of some plant "tea" a sediment forms despite the tea was filtered before. Solubility of various compounds and their mixes is very complex, quite unexpected behaviour often occurs.

 

[downwardsfromzero]

A possible sneaky trick when redissolving freebase into acid/vinegar is to put the powder in a funnel sat on top of a wad of cotton wool and slowly trickle the vinegar/acid through it. A dropping funnel would be ideal for this slow-dripping of acid onto the harmala base but it's not essential. This should clear up a certain amount of the annoying particulates without it being as much of a pain as filtering an actual harmala solution, which is often a complete pita nightmare.

 

[ChrisMMcD]

amount depends on amount of acid use, so hard to make a general estimate... just add slowly and mix well, first it will just neutralize the acid

I wonder why use acid at all when one can just boil harmala seeds in water and obtain the same decoction. I've tried that, and it worked well for extraction, just like for rue tea.
Could you please elaborate?
Thanks!

 

[Jagube]

I was separating harmine and harmaline for the first time in years and I think I messed it up.
After crashing out the harmine fraction with ammonia and collecting it, I proceeded to basify with lye instead of ammonia. It resulted in more stuff precipitating than should have. The extra precipitate is fluffy in solution and sticky after drying.

What would be the best way to clean it? Washing with more ammonia? Or do I need to do another Manske cycle on it?

 

[Transform]

I was separating harmine and harmaline for the first time in years and I think I messed it up.
After crashing out the harmine fraction with ammonia and collecting it, I proceeded to basify with lye instead of ammonia. It resulted in more stuff precipitating than should have. The extra precipitate is fluffy in solution and sticky after drying.

What would be the best way to clean it? Washing with more ammonia? Or do I need to do another Manske cycle on it?

Sounds like you can just redissolve the NaOH-precipitated portion in acid and repeat the ammonia process. Be sure to allow sufficient settling time after acidification in case any insolubles settle out.