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Yoda's instructions wrong ?

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Methrix:
I tried to extract the alkaloids from Mimosa Hostilis. (by Yoda's method)

I ended up with what should be the solvent (DCM) with alkaloids, but was a dark brown almost black thick muddy substanse, I don't know where it went wrong.

I started putting the crushed rootbark in an acid solution of pH 1, it was there for 4 days, the filtred bark was put in a new acid solution for about 10 days. I combined the two filtred solutions.

I've read that it was best to do a defat process as it would make crystals rather that an oily gel substans.
So i added the acid solution in my sep funnel, poured about 5-10 mL DCM within. Shaked and waited a few minutes.

Whats wrong ? I thought.
The DCM at the buttom was not clear but was thick an fatty. So my guess was that it probably was fat and i discarded it, and added more DCM, it was the same result. My conclusion : That how we do a defat.

So i made it alkaline with NaOH lye, my indicator strips, was miscoloured as the solution had become almost black, and i wished that i had bought a pH meter too. Well i stopped when i was almost sure with a pH 11.

I'm not sure but i think the solution was room temerature when i added it to my sep funnel.

I continued adding an equal volume of DCM in the funnel, shaked, shaked, and shaked. I took a nap, and went back couple of hours later, what i saw was the alkaline solution on top, and the layer below was the muddy substanse which i discarded at the tragic ending.

I really hope someone could tell where i went wrong, cause i have about 200mL acid with tryptamines (hopefully) left.

-Methrix

jsorex:
If you shake DCM hard, you have to wait REALLY long to get clear seperate layers. DCM goes to the bottom. It is the bottom layer, unlike naptha which floats on water. What went wrong? Why are you not pleased. Did you get active oil. Or are you not happy, because you didn't get crystals?

Dcm is effective but may pull other crap along. So take the black oil, and put it back in to acid water and do the entire extractio again with another solvent, naptha. Then wash with water.

-jsorex

gnrm23:
after agitating the basified solution with dcm, the alkaloids should migrate into the organic layer (dcm, bottom layer)... the goodies were in the last dcm, apparently discarded (?)...

don't you folks ever sleep?

Lysergic25:
SWIM always did many a naphtha run of the acidified solution to insure that all the plant fats and oils had been cleared away.  Then, when the solution was basified, there was hardly any gunk in the non-polar layer.

Maighstir:
I agree with the DCM comment. Use naphta, it works better with DMT extractions (at least for me; I only use DCM in final extractions, never in the first cause there's just too much shit in the mixture). Also, Yoda's method is perfectly OK.....for some plantmaterials. You must be carefull with extreme pH values cause some plants can give you a lot of trouble. If the pH is too low or high you could end up with thick gummylike mixtures because of the proteins present which precipitate. Some other plants will not do this, it's a trial & error process. The same problem could arise with other plantstuff (resins).

Vae victis meretrix est et mors venit.

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