• Members of the previous forum can retrieve their temporary password here, (login and check your PM).

syrian rue

Migrated topic.
I think there was a misunderstanding. I said there is 0 loss of MAOIs, harmine and harmaline. But of course that vasicine and vasicinone (and deoxyvasicine) are removed, thats the point of making a manske precipitation. But considering you have cleaned your harmalas from those alkaloids, you dont lose any significant harmala yield by repeating a manske (at least in my experience), and hence you are not losing harmalas when doing a manske in the first place, only losing the (usually) unwanted alkaloids
 
endlessness said:
I think there was a misunderstanding. I said there is 0 loss of MAOIs, harmine and harmaline. But of course that vasicine and vasicinone (and deoxyvasicine) are removed, thats the point of making a manske precipitation. But considering you have cleaned your harmalas from those alkaloids, you dont lose any significant harmala yield by repeating a manske (at least in my experience), and hence you are not losing harmalas when doing a manske in the first place, only losing the (usually) unwanted alkaloids
Did you ever actually measure yields?

You’d have to freebase and dry Manske-extracted alkaloids, then weigh them, the re-acidify, re-Manske, and re-basify. Dry and weigh again. There will definitely be some loss (some loss is unavoidable). The question is how much.
 
No I just dried the manske precipitation, weighed, redissolved them in hot water, re-precipitated with manske. And yeah I measured and yield loss was minimal, dont remember the exact numbers though. Try it out and let us know if you have different results. Also what you can do is on this second manske, add base to what is left behind and if there is any harmalas in solution they should precipitate as freebase (at least most of them). You can also theoretically do this to have your vasicine/vasicinone/deoxyvasicine separated to bioassay them separately if you want (though I dont see why one would, considering they arent MAOIs, unless you just want to know their effects for the sake of it or have a medical reason for it)

Do notice that if you re-basify the harmalas after redissolving manske as you propose, you will lose more alkaloids because harmaline freebase is slightly soluble in water, so you wont really be measuring the manske lost by itself. Hence why to know how much you lose with manske you need to compare it with only manske steps..
 
When weighing the resultant alkaloid salts from a Manske, you’re also weighing a certain amount of NaCl. I don’t know how much the NaCl content varies from extraction to extraction, but unless it’s removed, you can’t say precisely what your alkaloid yields are.

(Also, I’m sure you know that hydrochloride salts of alkaloids will have more mass than a molar equivalent of freebase.)

From what I’ve read, harmaline is practically insoluble in water, so loss of harmaline should be negligible when doing water rinses, especially if cold water is used.
 
Yes but if you use the same amount of salt for both saturations and the same amount of water you can expect it to be the same and it doesnt matter how much harmalas there are in comparison to salt impurities, no?

And yeah harmaline freebase isnt very soluble in water but it is a little bit. I have noticed in my tests definite loss of some alkaloids when base precipitating successively, definitely much more so than with salt precipitation, but I cant say for sure if its harmaline only that is loss or what. Im not sure about rinsing, Ive never done that.
 
endlessness said:
Yes but if you use the same amount of salt for both saturations and the same amount of water you can expect it to be the same and it doesnt matter how much harmalas there are in comparison to salt impurities, no?
I don't know.

I've never basified the leftover salt-water after a Manske. Have you? It would be interesting to see what the results might be, especially if done on 1st and 2nd Manske.
 
No Ive never done it but I remember reading a post of someone that did after the first manske and had many alkaloids crash, which I think are probably vasicine/etc, hence why I think it could be a good way to separate them if someone wants to bioassay them separately for some reason (though I dont see the need, and would advice caution if someone does, dont know how safe they are in concentrated big doses)
 
Hmm… Maybe another experiment?

I’m thinking of preparing a rue brew from 100g of seeds. Divide it in half.
Do an A/B on one half, and 2 or 3 Manskes on the other half, basifying the “waste” solutions.

Maybe next week or the week after?
 
gibran2 said:
endlessness said:
Yes but if you use the same amount of salt for both saturations and the same amount of water you can expect it to be the same and it doesnt matter how much harmalas there are in comparison to salt impurities, no?
I don't know.

I've never basified the leftover salt-water after a Manske. Have you? It would be interesting to see what the results might be, especially if done on 1st and 2nd Manske.
I have...it was a very interesting result, following a first manske

The first basification caused a precipitation of incredibly dirty alkaloids. In solution, they looked really muddy and formed some of the most bizarre clumps I've ever seen (they looked like the crystals, except brown and rather than being stars that had 7 or 8 spires sticking out, the clumps had flat edged planes sticking out where the spires would have been). I hope that makes sense, it's hard to describe.

Anyway, after doing another a/b on those precipped alkaloids, I removed a bunch of junk in my coffee filters and upon rebasification, I yielded crystals that looked remarkably similar to gibrans caapi copy xtals (these were the xtals I posted about in that thread). I suspected that these were the same xtals that mydriasis had encountered doing his a/b method, and this was confirmed when I tried to collect them and the kind of melted into my coffee filter.

I'm gonna re-dissolve and try to get those alks back and see if I can crystallize them a la gibran's thread, I'll post whatever I find.
 
Back
Top Bottom