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Harmalas yield

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FiorSirtheoir

FiorSirtheoir

Rising Star
Alright, used 50g of Syrian Rue, did a Manske process. Used sodium bicarbonate to seperate the harmine and harmaline, got a very small yield from the sodium bicarbonate, used KOH(Drip Lye) to precipitate the rest of the solution and got 4.5g after drying. Both the Sodium bicarbonate and the KOH were in liquid form. IS that much yield correct? What else could be in the harmalas? There where no other solids in the acid salt solution when the KOH was added.
 
what color is your extract? impurities may just come in the form of a decoloring, though after a manske the product should be reasonably clean... Could be though that with the KOH more impurities get caught in the product, similar to how it happens with caapi and sodium carbonate? Almost 10% yield sounds a bit high, but who knows. If your product appears to be light brown in coloring and not dark then I assume it's ok. The manske should have gotten rid of all unwanted alks... Did you wash often enough to get rid of the salt? You can easily test this by tasting your product to see if it still tastes salty.

that's all I got on ideas. Good luck.
 
Enoon,
It was a lighter colored brown. Washed it 3 times with warm water, keeping the pulled solution, now have about 1g of a darker tan. No salt taste at all anymore. NaOH seems to work alot better, second batch is gonna have more yeild. Though I probably lost a little the other night, when the harmalas was quite salty. Have 454g of rue seeds so I have plenty to play with. Wish I had a ph meter, I would just use the NaOH or KOH to pull the harmine. Enoon, what is your favorite spice tek?
 
Until yesterday, I’ve never done a Manske on crude Rue extract (I’ve done it on Rue extracted alkaloids). I must say that the Manske TEK is the absolute worst way to extract harmala alkaloids!

The crude extract contains so many impurities, that it’s nearly impossible to filter them. And since most of the impurities are insoluble, they can’t be separated from the alkaloid salts at all. And to get a reasonably clean product requires 3 or more runs through the TEK.

Here’s what I do, and it’s so much simpler and produces much better and cleaner yields in much less time:

1 – Do a simple A/B on the crude extract using NaOH. The alkaloids settle out nicely and can be easily separated.

2 – Re-acidify to remove insoluble impurities (of which there are many – much more than in caapi).

3 – Do a manske on the clean acidified solution to separate harmine and harmaline from other alkaloids.

4 – Basify resultant alkaloid salts with NaOH, rinse, and dry.
 
gibran2 said:
Here’s what I do, and it’s so much simpler and produces much better and cleaner yields in much less time:

1 – Do a simple A/B on the crude extract using NaOH. The alkaloids settle out nicely and can be easily separated.

2 – Re-acidify to remove insoluble impurities (of which there are many – much more than in caapi).

3 – Do a manske on the clean acidified solution to separate harmine and harmaline from other alkaloids.

4 – Basify resultant alkaloid salts with NaOH, rinse, and dry.
Click to expand...

cool, cool. But why basify as the final step? Isn't salt form better for oral use?
 
Apoc said:
cool, cool. But why basify as the final step? Isn't salt form better for oral use?
Click to expand...
I’ve always assumed (maybe incorrectly) that acetate salts of harmala alkaloids are hard to dry and keep dry (they’re hygroscopic I think). So the main reason is for storage. Freebase harmala alkaloids form a nice dry powder that is easily stored.

During preparation, freebase alkaloids precipitate out of solution and can be easily removed via decanting or filtration. Salts would need to be separated via evaporation, which would take much more time.

Also, when taking harmala alkaloids sublingually, it’s easy and convenient to take them in their freebase form. Some people also sprinkle freebase onto changa. And it’s very easy to convert freebase to a salt – just add a few drops of vinegar or other acid.
 
yes, the precipitation of manske is hcl salts, not acetate. Its only in acetate form when you dissolve with vinegar, but as soon as you saturate with salt, the Cl ion will attach to the harmalas forming harmalas HCl.

I noticed no degradation of harmalas, either in hcl and in freebase form, in glass vials in the fridge, after 1-2 years..
 
endlessness said:
yes, the precipitation of manske is hcl salts, not acetate. Its only in acetate form when you dissolve with vinegar, but as soon as you saturate with salt, the Cl ion will attach to the harmalas forming harmalas HCl.

I noticed no degradation of harmalas, either in hcl and in freebase form, in glass vials in the fridge, after 1-2 years..
Click to expand...
Ah yes, we were supposed to be talking about HCl salts, not acetates. :oops:

Don't HCl salts straight from a Manske contain lots of NaCl as well?
 
I made some mostly pure ones by under-saturating the solution with NaCL and letting it sit overnight. The next day, there were crystals grown on the bottom of the container. I decanted and and tasted some of the the crystals stuck to the bottom .They were wicked bitter and not discernibly salty.

I wonder if it would be possible to make mostly salt free Manske preciped harmalas by accurately controlling how much salt is left in solution.

I'm thinking, make a NaCl saturated solution (at room temperature) and add it to a small amount of well filtered rue tea.
Combine solutions, then reduce until the volume is exactly that of the original NaCl saturated solution.
Let cool to room temperature, perhaps overnight.
Poor off salt water.

It's been a while since I've played with harmalas. I think I'll put in an order for some seeds soon.
 
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