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A new level of harmala purity with this extraction

Migrated topic.
So this whack-job SWIM guy went ahead and:

-Basified with ammonia to around 11 or so until no more yellow clouds appeared.

-Janitorial strength ammonia was added 25ml first then 5ml at a time stirring and allowing to sit for 2-3 minutes between applications.

-Once alks had precipitated overnight and resulting liquid was no longer cloudy, the majority of the liquid was siphoned off then further decanted. Waste liquid was collected in a 1GL jar*

-Distilled water was added to the precipitant and allowed to settle before repeating siphoning and decanting 10 times. Waste water was added to 1GL jar.

-After the water began to run clear, precipitant was transferred to a 1/4pt jar and returned to an aqueous solution using a small amount of near boiling distilled water and just enough citric acid to dissolve all alks.

-Red liquid was filtered via coffee filters x2 before rebasifying with ammonia until clouds no longer formed.

-Decanted alks and washed once in jar with 20ml ammonia

-Decanted (from ammonia)again and allowed to air dry.


*The question or rather problem is that all seemed to go just as planned except that when put under a black light, the waste jar glows like a glow stick. Doesn't this mean that it still contains the alks. The red liquid glowed too but not like the waste water. Did he wash out a lot of the goods using the distilled water washes? Can this waste water be reduced and processed further?

The final product using this method turned out a fairly clean and smokeable powder that tastes like crap. Orally 120mg seems to be the dose and tastes only like good clean bitter alks.
 

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How does one extract with alcohol in the first step? Does one add it to the ground seeds and evaporate or does one cook the seeds with the alcohol and then evaporate? The rest of the tech seems simple enough but SWIM would like some clarification on this step.
 
christoadfur

Black light testing only indicates the presence of harmala alkaloids, not the amount. Dry harmine/harmaline hardly glows at all, even if it is pure. Only when put into solution does it glow bright, and pH also has something to do with how luminescent it is.

I'm sure there are solvents that will pick up the harmala alkaloids, but I haven't found them.
It's just an A/B extraction here, not all that confusing.
 
christoadfur said:
-Boiled in about 600ml of distilled water acidified probably too low (2.7) with citric acid for 40 min
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The reason it didn't work is because SWIY used citric acid.

If SWIY uses citric acid they cannot do a Manske extraction, it just doesn't work. SWIM has tried it, and it does not work.

If SWIY wants to do a Manske they must use either vinegar or HCL acid to acidify. HCL acid works better and faster than vinegar. Additionally, the extract should be reduced sufficiently to allow large crystals to form. Too much boiling down will caramelize your extract (bad) and not enough boiling down will result in small crystals.

Need to get it juuuuuust right. 😉

SWIM says if you get it right your liquid will become solid with crystals, like yogurt, if left in your refrigerator overnight.

The correct amount of salt to use is 1 gram salt for every 5 ml of aqueous solution. You can use as much vinegar/HCL as you want, there is no limit. Citric acid interferes with this kind of extraction, and should be avoided.
 
Ok I probably all ready know the answer to this. But SWIM has rue, put it in the coffee grinder, then the motor burnt out. Didn't like it at all. SWIM tried shaving up some of the seeds on his chopping board but it was getting everywhere.

How vital is the grinding of the seeds? Obviously it helps speed things up, but would a more patient extraction still yield good results? SWIM is currently soaking the rue in water after which he will freeze it to try break the stuff down a bit.

Would this help or does anyone have any better suggestions?

Hammer not available. :(
 
SWIM only tried with finely grinded seeds but he has heard a number of times people mentioning that its not necessary, that grinding finely is even bad because it releases more of the goeey stuff that makes filtering a pain. So maybe a patient extraction would work fine. SWIM would try it.

Btw, one very important part people (including SWIM) forget when doing the manske is to, before saturating with salt, DECANT the rue tea! This will make everything else after much easier because then this decanted 'junk' wont be mixed up with the alkaloids that precipitate
 
prey said:
christoadfur said:
-Boiled in about 600ml of distilled water acidified probably too low (2.7) with citric acid for 40 min
Click to expand...
The reason it didn't work is because SWIY used citric acid.

If SWIY uses citric acid they cannot do a Manske extraction, it just doesn't work. SWIM has tried it, and it does not work.

If SWIY wants to do a Manske they must use either vinegar or HCL acid to acidify.
Click to expand...

No. You just didn't give it enough time. You can use citric acid, or any other acid. Citric acid takes 2-3 times longer than acetic acid, but it works just as well, producing identical yields. Citric acid binds better to the alkaloids then acetic acid does, so you’ll need to give it more time to react with the salt, that’s all.
 
Swim have water solution of Harmala extraction made with citric acid. SWIM wants to use salt for participating alkaloids, and just wander if it'll be helpful if he add a little bit oh HCl beafore adding salt?

Logic: if Hydroclorides of Harmalinaes are insoluble in salty water then extra boost from HCl in soulution would speed up creation & participating Harmaline Hcl?

Is SWIM just crazy or, that have some logic?
 
Exarp said:
Swim have water solution of Harmala extraction made with citric acid. SWIM wants to use salt for participating alkaloids, and just wander if it'll be helpful if he add a little bit oh HCl beafore adding salt?

Logic: if Hydroclorides of Harmalinaes are insoluble in salty water then extra boost from HCl in soulution would speed up creation & participating Harmaline Hcl?

Is SWIM just crazy or, that have some logic?
Click to expand...

Adding HCl will speed things up a lot. Unless the HCl is food grade, I don’t see the point in contaminated the alkaloids with who knows what impurities are in the HCl. Why not just add the salt and wait for the citrates to form hydrochlorides from the salt (it will take a day or so)? I'm sure your citic acid and salt are both food grade.
 
SWIM have made a little experiment. He split his water solution in two parts, and in one add just NaCl.
In second one, he added 3 drops of preprepared HCl 1%.
There is no some special difference except that in second one, participation started faster a couple of minutes.
So...anyway, SWIM don't see some extra difference.
SWIM put both of them in fridge and he's going to sleep. Tomorrow will report is there any difference between participants.
If any.
 
Even if HCl is added to one and not the other, both should give the same results if enough salt was added to both of them and they have equal amounts of extractives and enough time is given for the alkaloids to precipitate. The citrates will just take a little longer because they need to form hydrochlorides first, that’s all.
 
Yes..but there is a little bit more kristal precipitated in second one. And faster. All integrades are food grade. SWIM just hope he didn't screw up the thing :(
Thanks Ron69

P.S

SWIM is interested in smoking his Harmalines. Is it necessary to freebase them (and how?) or it is ok to smoke them in hydrochloride form?
Is there any other way to clean the harmaline salts without repeating the process of salting?
Maybe insuflating would be OK? Does them burn the nose?
 
SWIM already did these tests long ago.

Citric acid, tartaric acid, acetic acid, hydrochloric acid, all work equally well but precipitate at different speeds when salt is added.

One thing, from what I've read, hydrochloric acid can precipitate the alkaloids on its own, without adding salt, if the solution is 30% hydrochloric acid.

The reason people use acetic acid is because it’s available in food grade form and the acetates are the most water soluble and the quickest to precipitate (besides the hydrochlorides). The acetates are extremely soluble in acetic acid.

The main reason people don’t use hydrochloric acid is because it’s very hard for the common person to get food grade hydrochloric acid, and also the hydrochlorides are not very soluble in dilute hydrochloric acid so extracting with hydrochloric acid is not a good idea.
 
whiterasta said:
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.
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Entropymancer said:
At pH 6, the harmine will be predominantly in the acid form, where it's water-soluble, while the harmaline will be predominantly in the freebase form, and should be relatively insoluble in water (I couldn't find a pKa for tetrahydroharmine).
Click to expand...
Harmine pKa: 7.70
Harmaline pKa: 9.80

I thought this would mean that harmine would precipitate out before harmaline, not the other way around?
 
OK, sometimes I'm a little dense. I know this is an old post, but I would like some clarification that I have been, as of yet, to get from this post.

For quite some time now, I have done a lazy man's crude freebase extraction. Rue is cheap enough, I didn't care about the extra cost of a little waste. I was able to get a Manske extraction to partially work a couple of times so, after forgetting to salt once I just started doing it the same way.

I realize it is VERY crude, but the process of trying too get a pure crystal was pissing me off repeatedly. So what I have been doing is this:

1. Put a hand full of Syrian Rue seeds in a pan.
(I have used ground seeds and unground seeds with little difference except that unground seeds produce more oils.)
2. Fill pan with about 3/4ths water and 1/8th (or more) vinegar.
3. Boil the seeds in the water & vinegar for about 1/2 to 3/4 hours, or until liquid is reduced to twice the level of the seeds in the pan.
4. Strain through tee shirt and set liquid.
5. Repeat steps 1.-4. about 4 more times or until the resulting liquid has little color to it.
6. Combine all the liquids saved and boil till reduced to about half of the pan.
7. Separate 4-6 eggs and through away the yolks.
8. Dump the egg whites into the boiling Rue liquid and stir until egg whites are fully cooked.
(It's weird, but it removes a lot of the oils.)
9. Strain through tee shirt and through away egg white crap (and I do mean crap).
10. Simmer remaining liquid to reduce to about 1/8 of the pan.
(At this point, when you turn off the heat things seem to further separate and kind of colonize in the liquid.
11. I place all this remaining liquid into a small scotch rocks glass and dump in some ammonia.
(It immediately turns baby poo yellow)
12. Let sit over night.
(By morning the liquid on top is clear and a bunch of brown gunk is on the bottom.)
13. I siphon off as much liquid as possible without disturbing the gunk.
14. Dump everything left through a coffee filter and squeeze out the liquid.
(This can be tricky to do without loosing the gunk but I've gotten good at it. A buchner funnel would be nice.)
15. Let the coffee filter with the gunk dry for a day or two.
(If I'm impatient I'll put it on a cookie sheet and in the oven on the lowest setting, occasionally chopping up the dust into finer powder.)
16. After everything is dry, I have a reddish brown dust that can be smoked.
(It is quite smokable by itself and can give a rather pleasant buzz in it's own right, but I know it could be a lot more pure. Also, goodness forbid, it is rather oily and when you put the flame to it, it is reduced to oils that boil and if you hit the pipe too hard those oils will travel down it and hit your lips. And you DO NOT want that to happen. It is THE MOST BITTER taste you could imagine. And if you swallow any, and maybe even if you don't swallow it, you will spew almost immediately.)

Anyway, this is what I have done for a well over a year now. I get good results when smoking it, but when I use it in a huasca, I still usually vomit, though not nearly as bad as I do if I just make Rue tea.

Anyway, I kind of wonder if someone could write out a step by step process that will yield what we see in the picture there at the beginning of this post. What I'm getting out of the beginning of the post is this (though I'm sure it is inaccurate):

1. Acidify alcohol with food grade phosphoric. (Vodka? No boiling required? What other acids would work?)
2. Grind up seeds and soak in acidified alcohol. (How long?)
3. Filter and set aside liquid.
4. Put seeds in new clean acidified alcohol.
5. Filter and set aside liquid.
6. Repeat 4. and 5. until it is "exhaustively" extracted.
7. Combine the acidified alcohol liquid that were set aside and evaporate until "alcohol is driven off".
8. Dissolve remaining extract in water.
9. Filter and keep what is in the filter. (I believe this is what he is saying. He says that Rue is red and Caapi is brown, and he describes the differences.)
10. Basify with ammonia. (And then repeat until ???)

Anyway, that's all the further I got to interpreting this. I'll try and edit and finish this later, but can someone clarify this please?



Also, did anyone else notice that WhiteRasa didn't really have too many more posts? Do you think perhaps he might have went on to perfect this method he was mentioning here and now sells the pure harmaline and harmine? Perhaps making some good money so no longer wanting to share the knowledge of how he got those nice crystals that seem to only come from vendors? Just wondering? Curios.


Further clarification desired: Are the harmala alkaloids soluble in alcohol in freebase form? Or in acid salt form? I know the oils seem to be quite soluble in alcohol after the fact because I can have rock hard baked on oils in my pipe and nothing seems to get that brick hard black crap. But it comes out VERY easily w/ a cotton swab filled with alcohol.
 
Also, did anyone else notice that WhiteRasa didn't really have too many more posts? Do you think perhaps he might have went on to perfect this method he was mentioning here and now sells the pure harmaline and harmine? Perhaps making some good money so no longer wanting to share the knowledge of how he got those nice crystals that seem to only come from vendors? Just wondering? Curios.
Click to expand...

Whoa there bud making some big assumptions,eh?:lol: I gave you folks the basics and you can't go from there? but then I HAVE been busy spending my mad cash from harmala sales:roll: .
It should be quite obvious what in my original experiment could be ommitted and what is integral.

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.

I do apologize for tossing the method out as lab notes rather than a recipe.However I make no other apologies.This was/is good original work and far superior to the "Manske" version.
I post here when it is relevant to aya, DMT, or beta-carbolines as
this is THE site for such. I however do most of my work in this using traditional methods so do not post just to rehash old subjects.I am presently here watching the progress of the cactus resin thread as it parrallels work being done on another forum more devoted to cacti.
I was quite suprised to see the petty assumption in this thread when I reviewed it.
Now it is laid out as simply as possible and I hope it helps those who found the original work too cryptic.
WR8)
 
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