I would like to thank (a lot) Gibran for the time to develop this simple and effective tek.
I would also like to make a contribution in the tek.
After the acidification step (mid tek) and decanting the yellow-brown supernatant, basification should be done drop wise with slow mixing of the supernatant. When pH is low (up to 3-6), addition of base dropwise will cloud it but it will dissipate, this should be repeated with calm and patience as the pH of the whole solution must equilibrate before adding more. When you reach pH 7-8 the first magic happens as the clouds do not dissipate, the whole solution will cloud up and very quickly brown-darkbrown precipitates will form, pH checking will show pH between 6-8, don`t go higher than this right now, it`s very easy to overshoot without electronic pH meters. Stop shaking and let it fall to the bottom.
Near this threshold pKa for harmine, a lot of it will drop out, some harmaline certainly drops out as well but way less. After solution clarifies the supernatant will continue to be light yellowish, meaning harmine-harmaline still dissolved. Also, at this pH brown harmine may precipitate cleanly giving you yellow-brown needles, brown precipitates after washing turn yellowish. A good sign, beautiful sight, specially because the crystals size will help it fall to the bottom quickly.
The yellow solution can now be basified further to drop harmaline and the rest of harmine out. Just keep slow mixing and dropwise add base, don`t overshoot! This makes the precipitates drop out too fast and become a powder which do not fall to the bottom. If this happens, reacidify dropwise then rebasify. Harmaline will drop out as white precipitates, if your pH is not very high (pH 9-10), white needles will fall out (they have a smaller length than the previous). Stop shaking, wait for the full precipitation to occur. Decant supernatant (that will remain somewhat yellowish but not fluorescent, you can try recovering whatever is in it by adding more base and putting it in the fridge, not much will come out).
Follow up with final cleanup until pH is 7-8 and you`re good to go. I suggest washing the precipitates with water pH 7-8 (just prepare a bunch using small amount of base), not plain tap water or distilled, as it it too acidic and you may dissolve crystals.
My contribution here is simple: do gradual pH increases on the basification steps and you get cleaner and bigger crystals that will speed up decanting and you can separate harmine and harmaline in a very visual way, stupid easy to execute. It takes more patience but turns out it speeds up further steps. Do not overbasify!If you add too much base at once, pH climbs too fast and alkaloids drop out instantly, resulting in a cloud that takes way too long to decant. Near the pKa, the alkaloids drop out slowly, sequentially adding themselves to precipitates making them larger.
Image shows unclean `harmine` to the left and `harmaline (+ harmine surely)` to the right. Further cleanup of harmine leads to yellow needles, takes little washes to get to it, since you didn`t add too much base at once. You can also wash once and readd acid (pH 4) to redissolve it, decant-filter brown gunk, then rebase it slowly to get the yellow crystals.
Ruffles attached the following image(s):
handh.jpg
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