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Topic Author Last Poster Posts Pages Last Post
Peganum Harmala Extraction FormulaDuke X PBeester 7 1 12-10-04  06:28 pm
Archive through November 29, 2004Duke X (Dukex)TehutiRoo (Tehutiroo25 1 11-29-04  11:23 pm

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Rio (Rio)
Senior Member
Username: Rio

Post Number: 891
Registered: 09-2004
Posted on Tuesday, November 30, 2004 - 02:56 am:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

My brew is still in the mail.
I can't wait to get started!
Please contribute your story, poem, black & white artwork....to the book I am writing about this community. See more information in General Discussions. Everyone will remain anonymous I will use your user name or an alias you pick out.
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philemon (Philemon)
Senior Member
Username: Philemon

Post Number: 448
Registered: 04-2004
Posted on Tuesday, November 30, 2004 - 07:02 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

hey, roo, this whole salt\rue thing you mentioned. I can't help but be very curious. is this a process to get pure harmine or something?
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TehutiRoo (Tehutiroo)
Intermediate Member
Username: Tehutiroo

Post Number: 55
Registered: 11-2004
Posted on Tuesday, November 30, 2004 - 11:46 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

From: http://www.erowid.org/plants/syrian_rue/syrian_rue_extraction2.shtml


Summary:

Take rue, powder it, place it water with small amount of acetic acid (distilled vinager) bring to simmer, cool and strain, repeat at least once, on the last batch, add the strained water hot and dissolve a good quantity of non iodized salt into the water, place in fridge/freezer (watch it so it don't freeze and break your container) and cool down to really cold, brownish orange flakes will percipitate out, let set in fridge until flakes settle to bottom, pour off excess liquid, then filter the rest through a coffee filter, wash with cold salt water, dry and scrape off the powder.

This is extremely efficient and I understand is the technique used in the field to test for harmaline.

From "The Alkaloids" Vol II (p393), Mankse:

"The crushed seeds of Peganum Harmala are covered with three times their weight of water containing 30 g of acetic acid per liter of water [white vinegar is about 50g / l or 5 %]. The seeds swell as they absorb the liquid and form a thick dough which is pressed after 2-3 days. The pressed seeds are once more treated as above with twice their weight of dilute acetic acid and, after maceration, the liquid is again pressed out. To the combined liquors, sodium chloride [that's table salt, man] (100g. / liter of liquid) is added to transform the acetates of harmine and harmaline into the hydrochlorides which are insoluble in cold sodium chloride solutions and are precipitated during cooling. The supernatant liquid is siphoned off, the crystalline residue filtered with suction and redissolved in hot water.

Addition of sodium chloride to the filtered solution causes the precipitation of the hydrochlorides as a crystalline mush and this process is repeated until the hydrochlorides have acquired a yellow color (for the purposes of this newsgroup, once is enough). The final product is then recovered by filtration."

Yield is about 4% of dry seed weight.

While this procedure is legal in the U.S. (where harmine and harmaline are currently unscheduled), it is illegal in Canada where harmine and harmaline are Schedule III. These are extremely potent alkaloids. Misuse of them can result in serious, even fatal, consequences. Read the info about MAO inhibitors.


Comments on this method by Dirk:

White vinegar contains 5 to 10% (5% is 50g/l), look at the label, dilute as appropriate. Say you want 500ml of 30g/l (=3%) starting with 8% vinegar you'd add 500x3/8 = 187.5 ml of 8% vinegar to 500-187.5 = 312.5 ml of water.

Supernatant is the liquid standing aove the precipitate. Pour as much as possibly off very carefully.

Well i tried it with suction on a buchner filter with a scintillated glass disk. Sound good no ? Well the filter clogged up immediately. There's still some red gum in there. Don't exactly remember how i got around this; possibly used a coffee filter (that ripped). Next time i think i would look for a finely woven cloth.

After dissolving it in hot water you can filter it again, collect the water and add the right amount of table salt. The amount of water to use should be minimal (minimizing loss because of the harmaline/harmine that doesn't precipitates), but not too little (loss through the amount of liquid that gets retained by the filter paper).

The paper {Hasenfratz et al., Ann. chim (10) 7,15l (1927)} then goes on to describe the separation of harmine from harmaline, but this procedure is slightly more complicated and not necessary for most purposes. The separation requires the use of a microscope and is based on the fact that when a warm aqueous solution of the hydrochlorides is alkalinized with ammonia, harmaline is liberated only after the decomposition of harmine hydrochloride is complete {harmine forms long needles; harmaline forms plates}). After separation the 2 salts are then further purified by recrystalisation of their salts.

I've found that harmaline and harmine are quite stable in acid solutions even at boiling water temperatures, however when the pH is raised to 11 or more boiling will rapidly remove the fluoresce of the solution (an indication that harmaline and harmine are being destroyed under these conditions).


Ann. chim (10) 7,15l (1927)

The separation of harmaline from harmine is based on the fact that when a warm aqueous solution of the hydrochlorides is alkalified with ammonia, harmaline is liberated only after the decomposition of harmine hydrochloride is complete. The appearance of harmaline is readily detected under the microscope since it consists of plates while harmine forms long needles. The addition of ammonia, therefore, is stopped as soon as crystals of harmaline are detected, the harmine is filtered off and the harmaline recovered from the filtrate by the addition of ammonia, The bases are then further purified by recrystallization of their hydrochlorides.


(discussion about this extraction procedure)
> ...My question is this: will this extraction actually work? I didn't think
> acheiving the HCl would be that easy! I've recently been thinking about how to
> conv

ert pure, crystalline, already-extracted freebase of a syrian rue extract
> into the HCl form, but that would be a lot of work (adding the right amount of
> moles to the right amount of harmala freebase--too technical), whereas the
> above method claims to extract the HCl directly from the acetic acid solution.
> I don't know too much chemistry, so pardon my ignorance here. All responses
> would be most appreciated!

I think the driving force for this reaction (the converting to the HCl salt) is the fact that the HCl salt is insoluble. Thus it seems to "disappear" from the right side of the harmaline-acetic salt <--> harmaline-HCl salt equation. So even if the dfisplacement of the acetate by the Cl is not favorable, giving an equilibrium concentration favoring the acetate, as the HCl salt crashes out of solution, the equilibrium will try and be maintained, forcing more of the HCl salt to be formed.

I do think this would work, but Id be careful not to add too much NaCl, or else you will get it crashing out as well when you cool. This will skew your yield and cause you to think you have more harmaline than you have. Cooling slowly may help this problem as well (keeping the solution supersaturated with NaCl instead of precipitating out).

psilo


Bilbo's Comments On Syrian Rue Extraction: (1996)

Do try to *defat* the potion while it is still in the acidic aqueous phase. You can then get rid of the oily residues then, then change the aqueous to a basic solution @ pH9 - 10, and multiply extract THAT into your non polar solvent; evaporate, and try. Be very conservative with measuring your dose. Anything over 100 mg. of extract should be aproached with caution.



(Message edited by tehutiroo on November 30, 2004)
Conventional thinking is the ruin of our souls,
something borrowed which we mistake as our own.
Ignorance is better than this; clutch at madness instead.
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jasontokes (Jasontokes)
Senior Member
Username: Jasontokes

Post Number: 418
Registered: 08-2004
Posted on Wednesday, December 01, 2004 - 12:48 am:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

thanks for that info , i have 454 grams of rue seeds, i'm going to get busy
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TehutiRoo (Tehutiroo)
Intermediate Member
Username: Tehutiroo

Post Number: 57
Registered: 11-2004
Posted on Wednesday, December 01, 2004 - 02:15 am:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

Do perhaps 30 - 50 grams the first time around.. if you make a mistake you will not lose all that much.
Conventional thinking is the ruin of our souls,
something borrowed which we mistake as our own.
Ignorance is better than this; clutch at madness instead.
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Duke X (Dukex)
Senior Member
Username: Dukex

Post Number: 646
Registered: 01-2004
Posted on Friday, December 03, 2004 - 10:35 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

"up for an experiment ?
when you're ready,
split it into two equal portions-
to one
add 1 tablespoon nonfat dry powdered milk. "


Ok this is done, the one on the right.

Upload

Peace...
'The Truth Is Out There'
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Hippie3 (Admin)
Board Administrator
Username: Admin

Post Number: 29577
Registered: 02-2001
Posted on Friday, December 03, 2004 - 10:37 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

are you going to let it sit awhile as roo suggested ?
how long, if so ?

Namaste


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Duke X (Dukex)
Senior Member
Username: Dukex

Post Number: 647
Registered: 01-2004
Posted on Friday, December 03, 2004 - 11:26 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

Yes until next weekend atleast.

Peace...
'The Truth Is Out There'
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Hippie3 (Admin)
Board Administrator
Username: Admin

Post Number: 29587
Registered: 02-2001
Posted on Friday, December 03, 2004 - 11:48 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

hmm,
i dunno,
milk can ferment so be sure to refridgerate

Namaste


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Duke X (Dukex)
Senior Member
Username: Dukex

Post Number: 648
Registered: 01-2004
Posted on Saturday, December 04, 2004 - 12:24 am:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

It will stay in the fridge.

Peace...
'The Truth Is Out There'
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Hippie3 (Admin)
Board Administrator
Username: Admin

Post Number: 29595
Registered: 02-2001
Posted on Saturday, December 04, 2004 - 12:28 am:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

i'd syphon the liquid off the sediment for the best possible taste.

Namaste


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Ferry (Spacecake)
Senior Member
Username: Spacecake

Post Number: 297
Registered: 01-2004
Posted on Monday, December 06, 2004 - 06:47 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

What about PH ?
If you finish the brew.. then your Ph will probably be low (ph 3-4).
If you ad some Soda to get the Ph at 7.....
will this have any affect on taste or storing(potency) ?
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Duke X (Dukex)
Senior Member
Username: Dukex

Post Number: 680
Registered: 01-2004
Posted on Monday, December 06, 2004 - 07:08 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

That is something I have started to think about myself.
Specifically where is the ph at the time of ingestion and
if by making it neutral would help the stomach.

I will test my ph this weekend when I taste this batch.

Peace...
"Courtesy Of The Red, White And Blue"
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Ferry (Spacecake)
Senior Member
Username: Spacecake

Post Number: 298
Registered: 01-2004
Posted on Monday, December 06, 2004 - 08:20 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

Good.. I'm not the only one thinking this..!

I will do the same thing here:

Ph from the first extraction is now (after filtering) 4.7
It was Ph 3.8 when I started brewing.

Second extraction is now boiling..

Post results later..!
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Hippie3 (Admin)
Board Administrator
Username: Admin

Post Number: 30450
Registered: 02-2001
Posted on Sunday, December 19, 2004 - 12:59 am:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

duke-
how'd this turn out anyway ?

Namaste


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Ferry (Spacecake)
Senior Member
Username: Spacecake

Post Number: 308
Registered: 01-2004
Posted on Sunday, December 19, 2004 - 11:29 am:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

Sorry guys... I'm not gone try this stuff any more...
Did have several experiments the last couple of years..and they were all failures.
I only get sick !
Did nothing wrong.. so I think I'm one of the few people were it just doesn't work,and I'm not dosing higher !!!
I'm just to care full....

Hippie: the milk thing did work for me..at least for the Viridis (did not taste so bad)
But when I added it to the Caapi ..it converted into little pieces ! yek....
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Hippie3 (Admin)
Board Administrator
Username: Admin

Post Number: 30504
Registered: 02-2001
Posted on Sunday, December 19, 2004 - 09:16 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)


quote:

Hippie: the milk thing did work for me..at least for the Viridis (did not taste so bad)
But when I added it to the Caapi ..it converted into little pieces ! yek....




hmm, mixed results.
wonder what the 'little pieces' that precipitated out of your solution actually were ??
milk can curdle, of course
or maybe it was the tannins.



Namaste


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Ferry (Spacecake)
Senior Member
Username: Spacecake

Post Number: 310
Registered: 01-2004
Posted on Sunday, December 19, 2004 - 09:32 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

I don't now what it was...!
It was pretty thick... more mass.. my English is to bad to explain.
I should have taken a picture !

Ph of the Caapi and the Viridis was the same.

Strange thing was :the Caapi extraction was clean ! (nice clear orange color)... the Viridis was not..very dark, lots of desicant !

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Ferry (Spacecake)
Senior Member
Username: Spacecake

Post Number: 311
Registered: 01-2004
Posted on Sunday, December 19, 2004 - 09:41 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

Caapi looked something like this: (before adding the milk)

Upload

After adding the milk ..but, up-side down !
(these are not the actual pictures ..but from my DMT extraction)

Upload

How can this happen ?

(Message edited by spacecake on December 19, 2004)
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Roo (Tehutiroo)
Member
Username: Tehutiroo

Post Number: 39
Registered: 12-2004
Posted on Sunday, December 19, 2004 - 09:57 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

You should not add milk to Caapi, no real reason. Brew up some Minosa extract then do the milk thing.
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Hippie3 (Admin)
Board Administrator
Username: Admin

Post Number: 30510
Registered: 02-2001
Posted on Sunday, December 19, 2004 - 11:17 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

my guess is we're seeing tannins & proteins binding and falling out of solution.
process should stop and settle down.


Namaste


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Duke X (Dukex)
Senior Member
Username: Dukex

Post Number: 744
Registered: 01-2004
Posted on Sunday, December 19, 2004 - 11:27 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

Hmm my brew looks nothing like that and is still in the fridge.
Will try and get it in before Christmas having a hard time giving
up the coffee this time of year.

Peace...


"Courtesy Of The Red, White And Blue"
www.woundedwarriorproject.org
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Duke X (Dukex)
Senior Member
Username: Dukex

Post Number: 764
Registered: 01-2004
Posted on Friday, December 24, 2004 - 03:20 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

Looks like the 12/26 is a full moon and may be the time for my brew. Wish me luck I will do a report when I get back.

Peace...
"Courtesy Of The Red, White And Blue"
www.woundedwarriorproject.org
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Redmonk (Redmonk)
Senior Member
Username: Redmonk

Post Number: 795
Registered: 10-2002
Posted on Friday, December 24, 2004 - 04:51 pm:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

Go for it Duke and good luck !!
Upload
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jasontokes (Jasontokes)
Senior Member
Username: Jasontokes

Post Number: 613
Registered: 08-2004
Posted on Wednesday, January 19, 2005 - 01:24 am:Edit Post Quote Text Delete Post Print Post Move Post (Moderator/Admin Only)

it is time.

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