Alkaloid Impurities

[DeltaSpice]

Hi, I need a bit of advise please.
I do many extractions of vine alkaloids . I smoke the vine Alks daily so I get through quite a lot.

My extraction method is the "Easy Caapi Vine Alkaloid Extraction Guide" (Gibran2) with a few modifications I have added over the years and on a larger scale.

Recently I made a mistake trying to rush.
The mistake is skipping step 3 "Remove Soluble Impurities".

If you don't remove the impurities (a darker liquid) and then Acidify, by the end of everything you are left with darker Alks, not fluffy at all and tasting bad. Unsmokable to me.

How can I remedy this?
I know it is hard enough to re dissolve this powder. Maybe hot fumaric acid solution?
But even then if I do get it dissolved , how could I purify my alks?

Thanks

 

[Sakkadelic]

Hi

It shouldn't be hard to dissolve this powder, white distilled vinegar and water should do it fast.

To clean it farther, you need to dissolve it in an acidic solution(white distilled vinegar works great), filter that, base with minimal amount of lye, let settle and decant(or filter), then do sodium carbonate or water washes until the water comes out almost colorless and your freebase will be very clean. On the last wash it would be better to use just water and filter or if you decant remove as much as you can water before drying.

 

[DeltaSpice]

Many thanks.
I had it in my head that once I had acidified the Alks that had a lye content there was no coming back .
Even though I used to do a double acidification back in the day so I should have known it would have worked.
When re dissolving Alks you have to make sure you use a dropper and form a paste.
Its all good now, my red vine Alks are looking pure white at the moment.
Thanks again

 

[blue.magic]

I also ended up with darker alks, just like you!

I have completely dissolved it in 3% vinegar, added 10% salt. I had some 12 grams of alks so I have used 1 500 ml water and 150 grams salt.

Unfortunately, nothing precipitated!

Now I freebased the alkaloids again, washed, filtered, dried and now will weight how much there actually is.

I am quite afraid these are companion alkaloids that don't crystallize from saline solution, but really hope I'm wrong...

 

[blue.magic]

After having no success with vinegar, I dissolved about 12 g of the dirty alks in 300 ml of 1% HCl, heated in microwave to near boiling and mixed in 30 g NaCl. Left to cool and sit at room temp. for 24 hours. You can see the pic of the salvaged crystals below. The harmalas are still very dirty so at least one more recrystallization is needed, then base, wash, filter, dry, enjoy

The crystallization took much longer than usual, even though lower concentration of alks crystallize almost immediately. This is probably due to lots impurities, mostly different alkaloids.

Note that crystallization is necessary to isolate the active alkaloids (harmine, harmaline) from the rest since all alkaloids will get through the simple cleanup steps.

After dissolving in acid, filter the solution well for better results.

 

[DeltaSpice]

Your talking about rue Alks I think.
Dealing with vine Alks is much easier.

I used to use Rue Harmala until my first experience with the vine. Then I knew I would never use Rue again..

Check out my pictures . Lovely white , red vine.
I also have some Ourinhos Als on the go. Probably the nicest of all the vines when smoked alone.