Rue extraction

[Kittynoggin]

Hello everyone,

I am attempting a variation on the tao of rue. (I think)
Anyways, I might have added too much vinegar as it reacted and foamed up quite a bit when I added the sodium carbonate. The instructions I have, say to keep adding the sodium carbonate until the solution becomes white. This never happened. I kept adding the soda until I ran out.
What I am left with had turned into a solid. Can anyone shed some light on what might have happened?

Thanks

Kittynoggin

 

[downwardsfromzero]

Sounds like you may have made a load of sodium acetate. Congratulations - you now have glow-in-the-dark hot ice!

Another possibility is that you (also) have a load of sodium bicarbonate, which is far less soluble in water. This can form by the reaction of carbon dioxide with sodium carbonate. And if you've used hard tap water, there's likely a bunch of calcium carbonate in there too.

You need to first obtain more base. It may be an idea to use sodium hydroxide at this stage, if you feel you can be trusted with that. Otherwise you can continue with the sodium carbonate - but dissolve it in water first!

Dissolve your current lump of solid in distilled water. It's likely there will be some insoluble precipitate remaining. Filter this off, or decant the solution away from it, and keep it for later. It may be some or all of the harmala alkaloids. Or if you used hard tap water, it may be mostly calcium carbonate.

Test the pH of the liquid (you know, the one you just separated from the solid). If it's pH8.5 or more your alkaloids are probably the solid that you've reserved. Even so, try adding a little more sodium carbonate (or hydroxide) solution to see if anything more precipitates. If not, your alkaloids are in the solid that you set aside.

If your harmalas are contaminated with calcium carbonate, separation can be achieved in at least two ways (not to mention via chromatography, but you probably don't want to do that yet). One way is to redissolve the solid in a sufficient quantity of acetic acid/vinegar and then to follow the Manske precipitation procedure with hot brine.

Another way is to dissolve the alkaloids in a solvent such as butyl acetate, followed by precipitation with citric acid.

Spoiler

By taking particular care with this dissolving process - for example, by filling the material into a column (such as a glass turkey-baster, plugged with a little cotton wool in the spout) and percolating the solvent through it - the alkaloids will dissolve in separate fractions. By careful collection of the percolation fractions a separation of the harmala alkaloids can be achieved without having to resort to careful pH monitoring as in the VDS protocol, for example.

 

[murklan]

By taking particular care with this dissolving process - for example, by filling the material into a column (such as a glass turkey-baster, plugged with a little cotton wool in the spout) and percolating the solvent through it - the alkaloids will dissolve in separate fractions. By careful collection of the percolation fractions a separation of the harmala alkaloids can be achieved without having to resort to careful pH monitoring as in the VDS protocol, for example.

I've never read that before! I don't really follow how to do it but will do some research. Thanks!

 

[downwardsfromzero]

By taking particular care with this dissolving process - for example, by filling the material into a column (such as a glass turkey-baster, plugged with a little cotton wool in the spout) and percolating the solvent through it - the alkaloids will dissolve in separate fractions. By careful collection of the percolation fractions a separation of the harmala alkaloids can be achieved without having to resort to careful pH monitoring as in the VDS protocol, for example.

I've never read that before! I don't really follow how to do it but will do some research. Thanks!

Novel research by me - a kind of "Poor Man's Chromatography" if you will. Also described in the Ethyl Acetate Approach for Harmala thread.

 

[Kittynoggin]

Thanks for the reply. I added some distilled water to the jar on the 31st. It is still solid, like I can't even chip it with a large metal spoon. I used a second pack of seeds and did more filtering. I got the acidic solution to turn yellow when adding the sodium carbonate. It settled and I decanted off the top layer. What was left was dissolved in hot vinegar and then 10g of salt was added per 100ml of solution. I let this cool and then put in the refrigerator overnight. The next morning I filtered and there was nothing in the filter.

I boiled the seeds from my first two attempts today. I'm going to try again. Maybe I added too much base the first time and not enough the second. We shall see.