I extracted 400g of rue seeds and I'm trying to separate the harmine from the harmaline, following the VDS protocol as closely as possible, but using tap water instead of distilled.

After 2 Manskes I dissolved the crystals in vinegar and then realized it wasn't necessarily, as water would have done the job and been preferable (less acidity -> less salts and less base needed for basing).
I divided the liquid in two equal amounts and put them in separate jars. I decided to do the VDS protocol on Jar 1 as it was, and do another Manske on Jar 2, dissolve the HCl crystals in water and do VDS on that.

Jar 1:
Around pH 8.5 I observed the first depression. But it was hard to measure the pH changes accurately as it fluctuated a fair bit and took a long time to settle. So I kind of gave up on exact measurements.

After basing to 10.8 I collected the 2nd precipitate, which was much less than the 1st, and a white layer formed on top of the liquid. I tried to remove as much as possible of the white layer, but I'm wondering what it is? Ammonia impurities? Salts in my tap water?

Jar 2:
I must have used too much salt in the Manske, because the harmala HCl crystals were contaminated with NaCl crystals at the bottom.

When I dissolved my crystals in water (roughly 350ml for 200g seeds), I was surprised that the pH was in the 3's
The 1st pH depression occurred around 5.5, it dropped to 4.3 and I left it to settle upon bringing it up to 5.8.

After 24 hours of settling, I was surprised to see that:
- The precipitate at the bottom of the jar was a mixture of brown(ish) and white(ish) bits, some of the white bits quite large.
- There were some needles on the walls of the jar (Manske crystals )
- A lot of brown particles were still suspended in the soup

I decanted the precipitate from the bottom and it separated into two layers: brown and white. Could it be that the brown stuff is harmine and the white stuff - harmaline?

Assuming all my harmine has been collected and the only alk left in the remaining soup is harmaline, can I base the remaining harmaline using sodium carb instead of ammonia?

Harmine is known to be darker in colour so brown should be correct.

See Phlux's Telepathine Tek for better reference.

This thread and this one too could come in handy.

Thanks Nereus, but the info under those links is obsolete and incorrect as was discovered by VDS and consequently discussed in this much more recent thread.

Also the fact that the 1st precipitate is brown doesn't necessarily mean it's harmine. It may be mixed with harmaline, and it may be that the impurities precipitate at a lower pH, giving the earlier precipitates a darker tint.

It is extremely easy to see whether separation is working by running TLC on the samples. Any chance you get that going? Def worth it for many different purposes.

You can also use mecke reagent at least to see if your harmine has significant harmaline contam since they react quite different:




Be well!

Yes, i am familiar with the VDS work thread.

I posted Phlux's in the hope that some picture comparison may be of help. Indeed his final product did not come out pure, but it's mostly harmine.

And great stuff endlessness, that can sure come in handy. Thanks for posting!

OK, thanks guys.

I'll look into TLC and maybe get a USB microscope as well.