A/B-extraction with vinegar, lime and limonene produces three layers

[harald25]

Hey!
I'm trying to do an a/b-extraction on phalaris, and I've run into an unexpected situation.
My procedure:

1) Harvest grass
2) Cut finely in blender
3) Add water and vinegar and boil for 30min (the vinegar will turn the DMT into DMT-acetate which is water soluble.
4) Filter out grass
5) Boil more so the chlorophyll coagulates. Filter through polyfill.
6) Add calcium hydroxide to the solution to basify (the DMT should now turn to freebase which is soluble in limonene
7) Add limonene and let sit for 20 min. Stirr several times during the 20 min.

At stage 6 two layers formed. The top layer was a light orange solution. The bottom was full of precipitates. Seems like the calcium hydroxide couldn't be dissolved properly?

I then added limonene to the solution and stirred well.
After letting it sit for a short while three layers started forming.
The middle layer is the same colour as the top layer from stage 6. The bottom layers is precipitates and the top layer is maybe the limonene(?) full of particles making it look alomst like the bottom layer.
After letting it sit for about 20 min, there seems to have formed a very thin layer at the top that is blank. This makes me think even more that the clouded top layer is indeed limonene with lots of impurities.

Now I'm wondering if I can collect the cloudy top layer and salt it with vinegar to get the DMT out of there?

 

[endlessness]

Where did you get the idea to use calcium hydroxide from?

You should NOT use calcium hydroxide for wet teks, only dry teks, since it´s not very soluble in water.

Now what I´d do is add some sodium carbonate so that it reacts with calcium hydroxide to form sodium hydroxide, which will help raising the pH. Then you proceed, getting the top layer where your alkaloids hopefully are, etc.

Next time please be sure to be informed on the process and chemicals use to prevent issues such as this.

Good luck and let us know how it goes!

 

[harald25]

I wasn't aware that calcium hydroxide is not very water soluble.
I only used it because I had read that it is less damaging for the environment than NaOH.

I will try adding sodium carbonate like you said.
Do you have any idea what amounts I should use?
I added 50g of calcuim hydroxide to my 900ml solution of 50/50 water and 7% vinegar.

 

[endlessness]

I´d add 50g of it in that case

 

[harald25]

I added 50g sodium carbonate, mixed it well by swirling thoroughly, and let it sit for 20 minutes. A lot less precipitates on the bottom, but still some. Is this leftover calcium hydroxide that didn't have any sodium carbonate to react with?
Or maybe calcium carbonate from the reaction?

 

[endlessness]

Not sure, you can try adding a bit more sodium carbonate, at least it wont hurt.. then proceed to remove the top layer and salt it.

As you may know, phalaris alkaloid content is very unreliable, so you may have dmt in your plant material in significant quantities, or you may not (same as for other alkaloids).. Hopefully you do have the goodies!

If you get something, when you bioassay, start with low doses.

Good luck!

 

[jamie]

this is common for grass extractions. A really hot heat bath(be careful!) with gentle stirring and then letting it cool and settle fixes it for me. Add some salt when it's hot also if you want.

 

[harald25]

When I continue tomorrow I will decant the top layer, and filter it.
I will then add more limonene to the filtered solution that remains, while having my glass jar in warm water.
The limonene layer that forms on the top will be decanted out into another vessel.
I will do a couple of pulls like this.
The pulls will be combined, and vinegar will be added.
I will decant out the vinegar into a new vessel, and add hot water to the remaining limonene solution. The water layer will be decantet out and combined with the vinegar.
This solution can be boiled down and hopefully will yield som stick dmt-acetate goo.

I intend to re basify this with sodium carbonate, and pull the now freebase DMT with heptane.
But only if I get enough sticky goo that I feel it's any point in doing it.

Pictures will be posted! =)