Cleaning harmalas with canola oil. Results-->White

[prottel]

Results from cleaning brownish caapi extract by dissolving it in canola oil at 150C, then crashing it out into the water layer with acetic acid. 250ml canola oil should be able to dissolve 1 gram harmine freebase and keep it dissolved at room temperature. Method also works for rue.

 

[Crystalito]

The purity, colorwise, is nothing short of impressive. When you heat the oil how much can you dissolve, have you taken any notes on how solubility increases with temperature? Also, do you think harmaline behaves the same?

A thing also to check would be how the solution would behave in freezing temperature...I wonder it if freeze precipitates...

 

[prottel]

The purity, colorwise, is nothing short of impressive. When you heat the oil how much can you dissolve, have you taken any notes on how solubility increases with temperature?

A thing also to check would be how the solution would behave in freezing temperature...I wonder it if freeze precipitates...

I tried dissolving 100mg harmine in 5 ml of canola oil at 150C. It dissolved just about all of it, but it took about 2 hours. When it was taken out of the oven, it started precipitating within a couple of minutes. I am not sure if freezing to precipitate it would work, as the oil would get very thick at those temperatures.

Also, do you think harmaline behaves the same?

I haven't tried it.

I have tried other oils, and it seems to be soluble in all of the oils I have tested.

 

[gibran2]

Incredible results! And now for the barrage of questions:

What is the yield?
Have you tried the product yet?
You say you used caapi extract, then you mention harmine: Which did you use?
How much vinegar did you use, how many vinegar washes, how much agitation?
How much oil per gram of crude extract?

Do you think dissolving the crude extract in vinegar first and then adding it to warm oil would work the same?

Very nice work!

 

[prottel]

Incredible results! And now for the barrage of questions:
What is the yield?

With the unclean caapi extract I only got ~35%. But when I used harmine cleaned twice through precipitation in water, I got a yield of 76% from 1 gram. But here is the thing. The yellow color that you see when you dissolve harmalas in water isn't the color of the harmalas, that is an impurity. When I dissolved the whitish extract in vinegar, the colour was much less pronounced than it is with regular extraction. So my thinking is that most extracts contains large amounts of impurities. Brownish extract probably isn't more than half actives, the rest impurities.

Have you tried the product yet?

Just dissolved some in acetic water. It is definitely active. But have not tried it in combo with dmt.

You say you used caapi extract, then you mention harmine: Which did you use?

I used an extract from FV. But I had cleaned it twice before, as FVs harmine is brownish in color.

How much vinegar did you use, how many vinegar washes, how much agitation?

I use 35% vinegar. To move it over to the water layer I used 2ml to be on the safe side, as 1 ml is usually enough to dissolve 1g harmine. Only did 1 wash, as the actives moves quite easily over into the water layer. A couple of minutes of agitation was enough. I did it while hot, but might work just as well with cold water.

Do you think dissolving the crude extract in vinegar first and then adding it to warm oil would work the same?

I tried it, but the impurities doesn't move easily over to the oil layer, just as it doesn't move easily from the oil to the water layer.

 

[gibran2]

So how much oil per gram of crude extract did you use, and how can you tell when all of the extract is dissolved?

I'm already starting the experiment - I put 1g of rue alkaloids in 40ml of soybean oil. At room temperature it will mix and form a muddy suspension. Does it clarify when dissolved?

Also, did you try lower temperatures? Do you think it would dissolve if the oil container was put in a boiling water bath?

 

[endlessness]

Awesome work Dagger! So my thinking was, one could grind rue, mix with calcium hydroxide or sodium carb, add water to make paste, dry, pull with hot oil (could try different kinds of oils), salt with FASW/Vinegar (maybe FASI/FASA?), then retrieve salt harmalas and freebase if wanted. This could potentially skip all the annoying harmala filtering when extracting rue (depending of course on how easy the separation of oil from rue and its filtering is in the first place).

What do you guys think?

Edit: though of course at least one manske salt saturation would have to be necessary to guarantee there was no vasicine/vasicinone, but could be done later on after its very clean.



I really want to test this but I dont think I have rue here. At least I might play around with purifying some crude extracts. Again, awesome testing there, the community expands and improves thanks to these good explorations

 

[prottel]

So how much oil per gram of crude extract did you use, and how can you tell when all of the extract is dissolved?

I'm already starting the experiment - I put 1g of rue alkaloids in 40ml of soybean oil. At room temperature it will mix and form a muddy suspension. Does it clarify when dissolved?

Also, did you try lower temperatures? Do you think it would dissolve if the oil container was put in a boiling water bath?

I would recommend about 250ml of oil per gram of extract. You may try a lower amount, but under 100ml probably wouldn't work very well, as it would only dissolve completely at a high temperature.

You can tell that it has dissolved when the oil clarifies. You should be able to see right through the glass when it has dissolved. It is best to try to mash the harmalas to as small particles as possible to help it dissolve. Otherwise the larger particles will fall to the bottom of the glass/jar.

It will probably dissolve in a boiling water bath, but I am not sure of the amount of oil needed. 250ml should be enough, but I think it will take longer time compared to 150C in an oven. Be sure to stir it around now and then to help with the process.

 

[Mydriasis]

If you still have the oil laying around you should try extracting from it 2 more times.

Interesting food-safe concept, never would have thought of that! The price of canola oil is pretty fair as well, so here's my thumbs up.

 

[prottel]

What do you guys think?

I think it is definitely worth a try. You may not need to filter the oil, just let the crudest particles settle, then pour the oil off and add acidified water. Most of the smaller rue particles may stay in the oil, while the actives move over to the water layer. The water should hopefully be easy to filter after this.

If you still have the oil laying around you should try extracting from it 2 more times.

Yes, I still have it. I may try a second extraction, but I did a very small scale test on my first experiment and there was barely any noticeable actives left on my second extraction.

 

[gibran2]

I tried this, and didn’t get good results. Of course, in my eagerness, I didn’t follow directions.

I weighed out 1g of rue extracted alkaloids and added them to 40ml of soybean oil. (Too little oil I assume.) I then heated it directly on the stove (didn’t measure temp., but I think it was at or near 300ºF), and most of the alkaloids went into solution (most, but not all).

I then added about 30ml vinegar. The vinegar turned deep yellow, as it usually does when extracted harmaloids. The oil was very dark brown. I removed the vinegar and did two additional plain water rinses of the oil. Both times, the water became slightly yellow. A separatory funnel would have come in very handy for this step!

I combined the vinegar and water rinses, then basified with NaOH. A tan precipitate immediately formed. FAIL.

I’m going to try again, using more oil, measuring the temperature of the heated oil to ensure it doesn’t go above 300ºF, etc.

 

[gibran2]

2nd try: Added 200mg rue extracted alkaloids to 50ml soybean oil. Carefully heated to 300ºF, stirring constantly. Most of alkaloids dissolved, giving a yellow coloration to the oil. There remained a small amount of reddish-brown granules that wouldn’t dissolve. The oil was poured off, leaving the reddish-brown granules behind.

Next, 40ml vinegar was added to the oil. The vinegar remained colorless this time! After stirring/agitation for a minute or so, the vinegar was removed. About 100ml water was added to the oil, stirred/agitated, then removed and added to the vinegar.

The aqueous solution was mostly colorless – maybe a very faint yellowish-green color. I next added about 2g NaOH dissolved in 30ml water to the aqueous solution. Nothing at all precipitated!?! FAIL again.

 

[SnozzleBerry]

Any possibility it's something unique to canola oil?

 

[Mydriasis]

I have a feeling it's the oleic acid working as the solvent. Which is also found in olive oil, etc.

 

[SnozzleBerry]

I have a feeling it's the oleic acid working as the solvent. Which is also found in olive oil, etc.

Cool...so aside from the new GM soybeans produced over at Iowa State, are there soybeans that contain oleic acid? If not, that could explain gibran's results, perhaps.

 

[gibran2]

I have a feeling it's the oleic acid working as the solvent. Which is also found in olive oil, etc.

Cool...so aside from the new GM soybeans produced over at Iowa State, are there soybeans that contain oleic acid? If not, that could explain gibran's results, perhaps.

I'll try again with 200mg alkaloids and 50ml of my expensive virgin olive oil.

 

[gibran2]

3rd (and final) try: 50ml extra-virgin olive oil and 200mg rue extracted alkaloids.

Yielded a yellow solution when vinegar was added (maybe pigments from olive oil). When solution was basified, a small quantity of brown precipitate formed. FAIL.

Either this technique doesn’t work, or it requires very specific conditions and/or oils/solvents (a specific type of oil, concentrated acetic acid, a specific base, etc.).

@ Dagger – are you sure the white powder is freebase alkaloid? How did you basify the vinegar solution? Is it possible the powder is a salt of some sort? Did you try dissolving it in water?

 

[Mydriasis]

Try burning some of the product with a lighter. If it bubbles and boils and smokes its probably what your looking for. If it just gets hot it's more than likely ionic, maybe sodium acetate.

 

[prottel]

Sorry to hear that you are not getting good results. Maybe it does not work so well with soybean and olive oil.

@ Dagger – are you sure the white powder is freebase alkaloid? How did you basify the vinegar solution? Is it possible the powder is a salt of some sort? Did you try dissolving it in water?

Pretty sure. I used lye to basify the vinegar solution. I dissolved it in water and as expected, it went into solution.


Here are some more pictures. The first is after moving 1 gram of harmine over into the water layer. The second is after freebasing(~650ml water).

 

[prottel]

Try burning some of the product with a lighter. If it bubbles and boils and smokes its probably what your looking for. If it just gets hot it's more than likely ionic, maybe sodium acetate.

I tried it. It burned quickly away and formed a liquid in the process, then shrunk and went dark. Did the same with the original harmine, same results.