Syrian Rue "intensive" extraction

[distopia]

Hello
It's my first post but I read the nexus since a while.

I use the Manske tech for Syrian rue, and I get a fairly good results.
4.5 - 5 % nice crystals.
I'v no problem with the tech itself. It's pretty simple, effective and a vacuum filtration system make all really easy.

Anyway:
This time I did not discharge the supernatant liquid as usual.
It was "apparently" exhausted. Meaning two salt saturation/cooling steps without any crystal.

But, careless, I try a step further.
I basify to 13pH with NaOh.

And now I'v got 3 layers.
Top: a smudge gray layer, layer not uv reactive.
Middle: a light dark-red layer, it seems the aqueous phase, layer light uv reactive.
Bottom: tiny deposit of a gray, smudge, substance, layer not uv reactive.

Anyone has some ideas about what I'v in my beaker?

Thanks

 

[distopia]

I can't believe none has ever try to utter basify the supernatant solution in manske rue tek...
Well, trying to catch some interest, I'll post a couple of photos and some hypothesis.

I started with 50gr rue seed.
I got, with plain manske tek, 3gr of dark brownish perfect crystal needles.
(3 salt/cooling pulls)
Then I basify the supernatant exhausted liquid with NaOh till 13pH.
Please note that, at this point, the supernatant liquid was still high UV reactive (just for this I decided to experiment)
Placed in freezer for some days, nothing happen.
Placed to room T° after 2-3 days I got 3 layers.

The bottom layer could be harmaline ( looks like "white sand" ), unlocked from the aqueous solution by the NaOH.
This could explain why the aqueous phase is a lot less UV reactive than before.

But I really, really don't understand the top floating layer
It seems a some kind of non-polar emulsion... but there's not non-p solvent in there.
Is there some kind of alk, in freebase, lighter than water??

Btw someone into rue extraction, would try this simple experiment too?
If the bottom layer will be hamaline, there will be a yield of 8-9 %... quite interesting indeed.

 

[endlessness]

the reason after manske people dont base it and discard that liquid instead (or try adding more salt and see if anything more precipitates) is because there are other alkaloids appart from harmine and harmaline which do not precipitate as HCL salts when adding table salt to the harmalas solution..

In other words, there are 2 alkaloids at least, vasicine and vasicinone, which most people consider undesirable, which AFAIK are not MAOIs and they have uterotonic and abortifacient effects, so it is specially dangerous for pregnant woman (and it seems very possible these alkaloids are associated in general with some negative side effects)

harmaline is not, because it would have come out together with harmine in the manske step

I would discard the acqueous layer, redissolve everything you have in fresh acidified water and start again with just manske, throw away liquid and forget about these other alkaloids.. but do as you please of course

 

[distopia]

In other words, there are 2 alkaloids at least, vasicine and vasicinone,

I well know about vasicine and vasicinone!
At the very beginning SWIM are used to take rue seed crushed in gel caps.
Really a bad thing. Just for this the need to move further to extraction.

Btw, in many years I'd never "really" seen this two tox alks.
And never though they could be in those layers!

harmaline is not, because it would have come out together with harmine in the manske step

I though It could be harmaline mainly for two reason:
- extraction are always not 100% efficient.
- harmaline concentration is quite correlate with uv glow, and the supernatant liquid always glows a lot
On the other side a yield of 9%... well it's really hard to believe, even for the best seeds strain. So should be something unwanted for sure.

do as you please of course

Thanks for the reply
Btw I never though to ingest something about those layer.
It was just an experimental play, I'm curious girl!

 

[mineatript]

New to Syrian Rue but you guys seem to know what you're talking about. I boiled 13G whole seeds in vinegar water five times to test out a kitchen tek I ran into. After filtration and basification, 24hr rest and refiltering per instructions I noticed the fluid I was supposed to discard still had a prominent greenish glow under black light. The same was true for the supposedly spent fluids in all the cleaning steps. Are harmine and harmaline the only alkaloids that glow or should I collect the supposed waste fluid for further processing. I don't want to throw the baby out with the bath water if I can avoid it. This may be the same question as above, just reworded. But I'm so new at this I can't tell for sure. I haven't even attempted a manske yet. Thanks for any response.