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A new level of harmala purity with this extraction Options
 
whiterasta
#41 Posted : 1/27/2010 12:09:39 AM

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"It seems that everything I knew was just a lie
A love, a hope, a dream, but what is that to you?
I can hold it in while I live, but it comes out when I die
The tragedy of truth, the liberties of lies
I see three sides to the coin as I flip it past my eyes
tossed from hand to hand you choose tails and I choose side."
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STS is a community for people interested in growing, preserving and researching botanical species, particularly those with remarkable therapeutic and/or psychoactive properties.
 
mumbles
#42 Posted : 2/17/2010 2:28:07 PM

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whiterasta wrote:
1)obtain a fat free clarified acidic extraction of the plant material.
2)basify using ammonia till no further precipitation occurs.
3)PATIENTLY wash the ultra-fine precipitate till wash is clear.
4)note color of precipitate, if brown while suspended, resalt, filter,rebasify, rewash. once should be plenty.
5)carefully isolate the F/B and dry and/or weigh and titrate to desired salt.
First off thanks for posting your results. Swim has a question, can any other base be used in place of ammonia, like say sodium carbonate?
 
SnozzleBerry
#43 Posted : 2/17/2010 2:47:03 PM

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I have done this tek with both ammonia and NaOH, they both work, I dunno about sodium carbonate, i'd assume so. Ammonia works great though, I see no reason to substitute, unless you don't have any...
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Vularin
#44 Posted : 2/22/2010 10:19:44 PM

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So is there a complete tek, with measurments and all of this one yet?
Its very vague to my limit chemistry skills...

thx,
V
 
endlessness
#45 Posted : 2/22/2010 10:33:20 PM

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SnozzleBerry wrote:
Ammonia works great though, I see no reason to substitute, unless you don't have any...


good reason to substitute ammonia: it stinks horribly!

sodium carbonate is sooo much nicer Smile

(each one to his own, though.. )
 
mumbles
#46 Posted : 3/3/2010 9:51:23 AM

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Entropymancer wrote:
So I've got a question: Why does the Manske extraction even exist? This works so much better, to extract, precipitate freebases as an off-white material, then proceed to clean up from there.
From swim's understanding there are a lot of alkaloids in syrian rue, some of which are pretty toxic or cause abortions and these are soluble in the saline saturated saline solution so manske wanted to separate those out and succeeded.
 
SnozzleBerry
#47 Posted : 3/3/2010 2:50:03 PM

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mumbles wrote:
Entropymancer wrote:
So I've got a question: Why does the Manske extraction even exist? This works so much better, to extract, precipitate freebases as an off-white material, then proceed to clean up from there.
From swim's understanding there are a lot of alkaloids in syrian rue, some of which are pretty toxic or cause abortions and these are soluble in the saline saturated saline solution so manske wanted to separate those out and succeeded.

yea, but whiterasta's tek handles those toxic nasties as well and is much simpler...which is what the essence of Entropymancer's quote was getting at...if they both remove the toxins and one is much simpler, why would people continue to use the other?

And endlessness, I feel you on the odor, it's definitely stinky, but it doesn't permeate the house or anything, so i didn't mind having to subject myself to that odor for the initial pour and five minutes it takes to decant...I have a bunch of sodium carbonate lying around (lye-ing around? hehe, i made an incorrect and bad chemistry pun) and ill give it a go on my current whiterasta extraction. I'm guessing i should just dissolve a bunch in water and slowly add the basified water, just as i would with ammonia?

SB
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mumbles
#48 Posted : 3/4/2010 10:35:57 AM

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SnozzleBerry wrote:
yea, but whiterasta's tek handles those toxic nasties as well and is much simpler...which is what the essence of Entropymancer's quote was getting at...if they both remove the toxins and one is much simpler, why would people continue to use the other, n'est-ce pas?
You'll have to refresh my memory, i thought it was just an a/b (or three) and freebased ALL the alkaloids.

whiterasta wrote:
1)obtain a fat free clarified acidic extraction of the plant material.
2)basify using ammonia till no further precipitation occurs.
3)PATIENTLY wash the ultra-fine precipitate till wash is clear.
4)note color of precipitate, if brown while suspended, resalt, filter,rebasify, rewash. once should be plenty.
5)carefully isolate the F/B and dry and/or weigh and titrate to desired salt.
 
SnozzleBerry
#49 Posted : 3/4/2010 2:36:47 PM

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mumbles wrote:
You'll have to refresh my memory, i thought it was just an a/b (or three) and freebased ALL the alkaloids


yes...I'm not sure where you're hung up. The toxins in rue are not alkaloids (not to my knowledge anyway). The main alkaloids in rue by % composition, to my knowledge, are harmine and harmaline. Erowid states that rue contains Harmine, Harmaline, and Tetrahydroharmine (I hadn't known rue contained THH, maybe in very low quantities or something like that). So, yes, the method you posted is whiterasta's tek and it does freebase the alkaloids. The toxins are removed via the alcohol soak, just as with cold water or alcohol extracts from countless ethnobotanicals. The reason people even bother with these simple extractions is because they separate the goodies from the nasties. Otherwise we'd probably see many more people just eating the plant material. Hope that makes sense/helps you out.

peace
SB

EDIT: well, I guess technically the goodies are removed via alcohol soak, and the toxins and inert plant material are tossed, but you get my drift...
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endlessness
#50 Posted : 3/4/2010 2:56:11 PM

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SnozzleBerry wrote:
mumbles wrote:
You'll have to refresh my memory, i thought it was just an a/b (or three) and freebased ALL the alkaloids


yes...I'm not sure where you're hung up. The toxins in rue are not alkaloids (not to my knowledge anyway). The main alkaloids in rue by % composition, to my knowledge, are harmine and harmaline. Erowid states that rue contains Harmine, Harmaline, and Tetrahydroharmine (I hadn't known rue contained THH, maybe in very low quantities or something like that). So, yes, the method you posted is whiterasta's tek and it does freebase the alkaloids. The toxins are removed via the alcohol soak, just as with cold water or alcohol extracts from countless ethnobotanicals. The reason people even bother with these simple extractions is because they separate the goodies from the nasties. Otherwise we'd probably see many more people just eating the plant material. Hope that makes sense/helps you out.

peace
SB



yes there are unwanted alkaloids, vasicine and vasicinone.. I know for a fact they do not precipitate with manske, hence the great advantage of manske, but I do not know if they are removed by whiterasta's acidified alcohol... so until I know that, I will preffer doing manske at least once during the process
 
SnozzleBerry
#51 Posted : 3/4/2010 3:14:51 PM

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There are some articles at Science Direct, that I can see from the preview talking about the degradation of quinazoline alkaloids...From the preview/google cache it looks like it's saying somethin about degradation of vasicinone around pH 4, but my school subscription is acting funny and won't let me open the articles. I dunno if it's truncated and just grabbed 4 from something else, but I'm gonna keep trying to get in, as that would be good to know. If this is the case, then acidifying low enough with this method would handle those unwanted alks. Although personally, as someone who used to eat a gram of seeds occasionally and having done manske, even if those alks are still present, overall its nowhere near as bad as the seeds and nowhere near as time consuming or intensive as manske. I'll post what I find if my account stops acting weird...or better yet, if someone else has access to science direct and can check, that'd be awesome.

peace
SB
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endlessness
#52 Posted : 3/4/2010 4:20:13 PM

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yeah would be interesting to know about it, but remember, its also important to know not only that it degrades, but what it degrades to.... Who knows might have even more unwanted

Also, I guess you are a man, right? me too.. I've heard that women seem to have more trouble with quinazoline alks..

Btw, I dont understand why people say manske is 'time consuming'... It is very easy, in 20 mins all the alks have precipitated (I tested myself and there was no late precipitation).. The filtering can be helped if the brew was filtered thoroughly before precipitating, or anyways if you dont like filtering you can just leave standing a while and decant, and redissolve last bit again for the later base precipitation.. Each one to his own of course.. Smile
 
SnozzleBerry
#53 Posted : 3/4/2010 4:28:20 PM

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yea, I'm a man, its probably the same for all of the uterine contracting stuff, like lsa/lsd and whatnot, harder on women easier on men due to the whole biological differences for makin babies Wink

As to time consuming, i find it to be comparatively longer/requires more overall involvement and observation. For certain things that i'm not truly fascinated with or overly interested in, i like to have things that i can fit easily into my rather hectic schedule and find that this method does that. But i agree, to each their own, it is from our diversity of methods that we can truly accumulate the most comprehensive knowledge about what's going on...
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mumbles
#54 Posted : 3/5/2010 2:27:46 AM

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SnozzleBerry wrote:
The toxins in rue are not alkaloids (not to my knowledge anyway). The main alkaloids in rue by % composition, to my knowledge, are harmine and harmaline. Erowid states that rue contains Harmine, Harmaline, and Tetrahydroharmine (I hadn't known rue contained THH, maybe in very low quantities or something like that).


These are the alkaloids in Syrian Rue seeds:

Peganine (Vasicine)
Harmalol
2,3 - Trimethylene-4-quinazolone
1,2,3-(a-Hydroxy-trimethylene)-4-quinazolone
Oxodeoxypeganine
Oxopeganine
Tetrahydroharmine
Deoxyvasicone
2-Alkoxy-4-quinolone derivative
Deoxypeganine
Peganidine
Pegamine
Peganol
Ruine (8-Hydroxy-glucosylharmine
Deoxypeganidine
Dipegine
Isopeganidine
Vasicinone
Dyhydroruine (8 -Hydroxyglucosyl-harmaline
5- Hydroxytriptamine
6- Hydroxytriptamine
Harmol
 
SnozzleBerry
#55 Posted : 3/9/2010 1:18:06 AM

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yea, but in what minuscule concentrations?
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burnt
#56 Posted : 3/9/2010 8:22:05 AM

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doing the salt precipitation method yields only harmine and harmaline in detectable quantities. the other extract method being discussed here has not been analyzed yet.
 
SnozzleBerry
#57 Posted : 3/9/2010 2:47:41 PM

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burnt wrote:
doing the salt precipitation method yields only harmine and harmaline in detectable quantities. the other extract method being discussed here has not been analyzed yet.

well...does someone with the analytical machinery have the time or interest in seeing what this extraction yields? I, and I'm sure many others, would be very interested in seeing just what whiterasta's method pulls. I've been using it over manske for quite a while and have been more than happy with the results, but I'd love to see a breakdown of what we're actually pulling with this.

peace
SB
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T
#58 Posted : 3/12/2010 8:01:08 PM
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whiterasta wrote:
This method using phosphoric acid gives a highly separable salt of harmaline (almost insoluble in concentrated solutions) which will precipitate as needles far sooner than harmine and can easily be filtered off for separating the alkaloids.


Whiterasta could you explain this in detail?
Freebase is very hard to deal with (it runs through every filter).
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soxy bastard
#59 Posted : 3/12/2010 9:58:44 PM

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SnozzleBerry wrote:
burnt wrote:
doing the salt precipitation method yields only harmine and harmaline in detectable quantities. the other extract method being discussed here has not been analyzed yet.

well...does someone with the analytical machinery have the time or interest in seeing what this extraction yields? I, and I'm sure many others, would be very interested in seeing just what whiterasta's method pulls. I've been using it over manske for quite a while and have been more than happy with the results, but I'd love to see a breakdown of what we're actually pulling with this.

peace
SB


Paper chromatography under UV-A with rue shows two major bands and one minor trace band
Similar using Caapi yeilds three main bands and no trace band.
ethanol water extract yeilds up to seven flourescent bands and several visible light markers for rue
similar for caapi yeilds four to six flourescent bands and several obvious tannin markers.
No other analysis has been performed in the wake of the chromatographic match for harmine and harmaline standards for both rue and caapi, however in the abscence of a THH standard it is only assumed the third band found in caapi extract is THH
I am satisfied this method is selective as the manske route within the parameters of crude analysis performed along with selective precipitation from rue F/B yield only harmine and harmaline with the leftover solution nearly devoid of any alkaloids.
Research on whiterasta indicates a past professional carreer in chemistry. And in reading much of his work from the shroomery to the nook he posts in scratch pad lab note form expecting any who read to automatically be up to speed on where ever his mind has wandered.That said in each case he has put forth a tek it has proven itself from introducing KOH in reducing emulsions,this F/b precipitation to what he has shared with chinacat @ the shroomery on the 70's acid scene has been spot on.
I expect he considered the removal of unwanted alkaloids by way of acidifying the menstrum followed by rapid raising the PH having a similar effect as the acidic extraction and halide substitution.
SB
 
SyZyGyPSy
#60 Posted : 2/22/2011 6:08:11 PM
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I know this is an old thread but I feel compelled to jump in and say that after doing a Manske NaCl precipitation on an acidified aqueous harmala extract, once the precipitated harmine/harmaline have been removed by decanting/filtering, the remaining solution can be basified (and yes, sodium carbonate is my favorite for this, just watch out for the volcano), and more alkaloids will crash out. They are darker in color and are not harmine and harmaline, they are all the other alkaloids - or degredation products thereof - that are present in harmala.

Presumably the makeup of these alkaloids varies due to genetics, growing conditions, time of harvest, etc.

Point is, there's other stuff in rue besides harmine/harmaline, and the manske NaCl precip separates these. I don't know about whiterasta's tek cuz it uses alcohol, and he never really clarified that part about preciping harmaline salts at pH 6 but it sounds to me like there's at least a possibility that this could extract those other alkaloids.

The way to find out for sure would be to do a whiterasta tek, then redissolve in acidic aqueous solution, do a Manske NaCl precip, remove harmine/harmaline crystals, then basify with sodium carbonate (or lye, ammonia, or whatever, though ammonia fumes are harmful and lye is dangerous so why not sue sodium carbonate when all you gotta do is bake baking soda?). If anything else crashes out, then we know this tek does not isolate pure harmine/harmaline.

I agree, whiterasta's a knowledgeable dude, but we all tend to overlook things sometimes. And he never did really clarify the tek (not pointing fingers here, I've promised to post many things that I still haven't gotten around to... just saying).

Love,
SyZ
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