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[Work Space] No filter, No reduce Syrian Rue Extraction Options
 
wearepeople
#1 Posted : 5/13/2015 11:43:02 PM

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Hi All,

This is a workspace, so please don't use this as a TEK unless you're down to experiment and post results. It's still in the making.

EDIT: Skip over all this chat log and get right to the good post: Ouro Explains The Process.

Essentially I heard little bits in chat that a simple way of extracting Syrian Rue came about. Dreamer042 explains:

Quote:
make rue tea, *don't reduce*, base it out, collect precipitate, either wash well for use as is or dissolve in acidic water and base again to clean, or manske to isloate harmalas from other alkaloids and base again, repeat dissolve in acidic water and base as many times as necessary for desired level of purity


Ouro says:

Quote:
00:47:25 ‹ouro›looks perty good
00:47:38 ‹ouro›i think i got some original inspiration from mydriasis
00:47:43 ‹ouro›so make sure to credit him
00:48:23 ‹dreamer042›lol ouro trying to pass the buck I passed to him
00:48:33 ‹ouro›make tea -> base immediately, let settle enough to safely discard most of the water without losing precip -> redissolve in acid -> settle in fridge -> manske or rebase and wash
00:48:51 ‹dreamer042›^^^^
00:48:52 ‹dreamer042›post that
00:49:25 ‹ouro›for base washing instructions: you will end up with precipped harmala in basic water at some point, with dissolved lye/soda carb/tsp/whatever base
00:49:33 ‹ouro›it will probably be around ph10
00:49:42wesker joined the room
00:49:52 ‹ouro›a 10:1 dilution of this water will result in an approximate drop of 1 ph
00:50:22 ‹ouro›so to reduce the ph from 10 to 7, removing 90 percent of the water and replacing it with fresh water 4 times should be sufficient
00:50:29 ‹ouro›at that point the whole thing can just be evapped
00:50:54 ‹ouro›WARNING: if you miscalculate or do this process loosly you will end up with base in your harmala product
00:51:39 ‹ouro›oh yeah, it might be wise to filter after settling in the fridge in the acid phase
00:52:43 ‹ouro›but it will be much easier since most gunk is dissolved in the tea you threw out initially after precipping the harmala
00:52:47 ‹ouro›thats aboot it



For more detail read this:
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Good quality Syrian rue (Peganum harmala) for an incredible price!
 
Infectedstyle
#2 Posted : 5/14/2015 12:25:44 AM
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No filter, No reduce Syrian Rue Extraction

YESSS
 
wearepeople
#3 Posted : 5/14/2015 1:15:22 AM

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To read more Chat Ramblings about the process:

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DreaMTripper
#4 Posted : 5/14/2015 3:58:58 AM

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Seems a good idea to me filtering is a tedious process as is decanting which I found the most troublesome as every time I would move the jar to separate precips from liquid the precips would swirl around making it very difficult to separate.
You could even do it without heat and just let them sit (unground) in acidic water for a week shaking them regularly. This could reduce the gunk that ends up in solution.
 
ouro
#5 Posted : 5/15/2015 1:27:09 AM

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I suppose I ought to just lay this out clearly:

Principals: Harmala alkaloids in the seeds of peganum harmala are readily soluble in water. They are practically insoluble in basic water, and very soluble in most types of acidic water.

so the basic principal is: discard all solids in when your material is acidified, and discard all fluids when it is based.

Step 1: get the alkaloids into tea solution.

There are many strategies people have used with success for this. I think someone showed that PCing whole seeds for 2 hours nearly exhausted them. Most people just boil them, either ground or whole. I freeze/thaw them once or twice and boil them whole personally. One way or another you want to dissolve the alkaloids into a tea. Usually 2-4 pulls are used.

step 2: purify your tea.

2.1: By far the easiest way I have found to do this is to boil the seeds in water for about an hour, remove the water, and immediately base this water. The harmalas will precip immediately. Let them settle until you can safely pour most of the water off without losing any of the precip. This water you are pouring away contains most of the gunk that would be concentrated when reducing and then proceed to make filtering extremely difficult. Do this for each successive boil and you can see how much yield you are getting and when it is no longer worth it to you to continue making tea. Collect all these precips. You can do an optional preliminary wash of these freebase harmalas by adding some water, letting them settle, and removing most of the water again. Then, dissolve them all in acidic water.

2.2 Let this acidic solution settle in the fridge. There might be some gunk - discard that. This is an opportune time to filter, but it is not necessary.

2.3 optional Manske if you feel like it. I omit this step. It makes pretty crystals but I have no issues with the minute amount of vascicine and related alkaloids and the extract I get without manske is clean enough for my purposes.

2.4 optional successive base/acid washes. You can base the acidified harmalas and discard the water, wash with clean water, re-acidify, filter out solids, then rebase etc to your hearts content. I find that if the other steps are done carefully this is not necessary.

step 3: retrieve your alkaloids. If you manske'd you can pretty conveniently collect harmala hcl crystals.

This is my preferred collection tactic:

Starting from precipped harmala freebase in basic water: this water is probably around ph 10 or 11 if you based carefully. If you added too much base you can do this process a few extra times to clean it out. A 10:1 dilution of the water will result in an approximate drop of 1 ph. So, removing 90 percent of the water, refilling it, letting the precip settle, remove 90 percent of the water, etc 4 times should wash the excess base out. In practice you probably want to do this wash 5-7 times. The harmala freebase buffers the solution and keeps the ph above 7; however, you can use this principal to estimate how much dilution is necessary to remove the excess NaOH, TSP, sodium carbonate, whatever base you used. Once you have washed out the excess base, evap the whole mess and scrape up the harmala freebase powder without having to filter.

Alternately you can try your luck filtering the freebase, washing it, drying it, and removing the freebase from the filters. If you have a vacuum filter setup this is probably easier to do than the above washing and evapping technique.

enjoy
 
wearepeople
#6 Posted : 5/15/2015 3:05:17 AM

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Yay!

It works! 5 hours from beginning to completely dry harmalas/other. If you're concerned about "other" please see this post.

I did acid->base twice, no manske, started with 204g syrian rue. Yielded around 3g of powder. The powder is a light-brown color; it looks very similar to ground cinnamon or cacao powder.


If you want to see the details of what I did click this:

wearepeople attached the following image(s):
Untitled.jpg (199kb) downloaded 1,752 time(s).
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slewb
#7 Posted : 5/15/2015 3:29:19 AM

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Haha I remember the first time I tried to filter rue - I was not having any of that Wut?. I generally just do Gibran's guide with a few manskes thrown in somewhere along the line (which as far as I can tell this basically is). Saves a lot of frustration.
 
DreaMTripper
#8 Posted : 5/15/2015 10:05:31 AM

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It is basically gibrans tek without filtering, that doesnt seem a good yield wearepeople from 204g of seeds I would expect at least 6g..
 
wearepeople
#9 Posted : 5/15/2015 3:40:26 PM

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YES! This basically is Gibran's Tek but with one major difference: DON'T REDUCE/COMBINE THE ACID BOILS! BASE THEM IMMEDIATELY! Something about reducing the liquid seems to make the gunk in Syrian Rue coagulate and become a pain for the rest of the process.

DreaMTripper wrote:
It is basically gibrans tek without filtering, that doesnt seem a good yield wearepeople from 204g of seeds I would expect at least 6g..


Indeed, very poor yield. From 204g I would expect waaaaay more than 3g, something on the order of 10g (5%+). I was going for as fast as possible, not as thorough as as possible, hence only 2x boils, one at 44 minutes then 24 minutes. During the base precipitation steps, I barely waited at all for precipitation to form; as soon as I saw a layer, I siphoned off the rest and dumped it.

Also, I used sodium carb as the base. In the past I've used NaOH as the initial base and sodium carb for the last base. NaOH seems to do a better job.

For those of you unfamiliar with Gibran's Tek it can be found:
here
with the original thread here
And posts where Gibran discusses using his/her Tek on Syrian Rue:
here
here



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ouro
#10 Posted : 5/15/2015 7:18:07 PM

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It's hardly a 'tek' in the first place. its 3 steps you can do in any way you find convenient: make tea, purify, retrieve alkaloids. The only difference here is a few pointers that ime and a few others make it much less time consuming and frustrating. Basing immediately after making tea, and Dreamers addition of using a siphon, etc can make the process much more attractive.
 
DreaMTripper
#11 Posted : 5/16/2015 9:58:34 AM

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Fair enough, I suppose you can always retrieve the remaining ammount later at your leisure.
 
DreaMTripper
#12 Posted : 5/24/2015 10:43:55 AM

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If youre not concerned on getting the most out of every seed seeing as rue is so cheap then how about just half filling a jar with seeds then covering with vinegar water, say up to 3/4 jar leaving room for sploshing about then just frequently shake rigorously you could even leave it in a heat bath and/or ontop of a radiator.
Decant liquid and add a base to precipitate. Decant liquid away and wash/reacidify then base or manske accordingly.
 
wearepeople
#13 Posted : 5/24/2015 6:50:51 PM

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DreaMTripper wrote:
If youre not concerned on getting the most out of every seed seeing as rue is so cheap then how about just half filling a jar with seeds then covering with vinegar water, say up to 3/4 jar leaving room for sploshing about then just frequently shake rigorously you could even leave it in a heat bath and/or ontop of a radiator.
Decant liquid and add a base to precipitate. Decant liquid away and wash/reacidify then base or manske accordingly.



I think I'll give that a try. Sounds like my kind of extraction. "Set it and forget it" just like the Ron Popeil's Ronco Rotisserie ads.
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geeg30
#14 Posted : 5/25/2015 5:12:44 AM

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You don't have to basify immediately. I use this type of method for my extractions and have had no problems combining my pulls then basifying. I get around 5g crude from 100g seeds. I also don't bother with reacidifying as a couple of washes seems to do the trick.
Here you!!! Gonnaenodaethat

"Iceberg???? - What Iceberg????"
 
DreaMTripper
#15 Posted : 5/25/2015 12:28:31 PM

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wearepeople wrote:
DreaMTripper wrote:
If youre not concerned on getting the most out of every seed seeing as rue is so cheap then how about just half filling a jar with seeds then covering with vinegar water, say up to 3/4 jar leaving room for sploshing about then just frequently shake rigorously you could even leave it in a heat bath and/or ontop of a radiator.
Decant liquid and add a base to precipitate. Decant liquid away and wash/reacidify then base or manske accordingly.



I think I'll give that a try. Sounds like my kind of extraction. "Set it and forget it" just like the Ron Popeil's Ronco Rotisserie ads.


You would have to filter but you could just do it through a t-shirt and save the remaining seeds for a later date, I have no idea how many g you could fit into a jar (depends on the size I suppose!) but the idea is to forget about maximum yeild per pull and efficiency and go for saturating the liquid with the harmalas in salt form to get a quick extract then you could leave the liquid aside after the first collection to precipiate whats left.
so
1. fill large lar 2/3 to 3/4 with seeds
2. cover in vinegar water plus a bit more leaving say 1/8 jar for fee space for movement
3. shake like your life depends on it whenever you can over a few hours
4. leave in a heat bath for a couple of hours
5. drain liquid through t-shirt into another jar
6. add highly basic solution ph12 dropper wise until clouds precipitate
7. collect full spectrum whichever way you see fit
Now you could either a) diossolve in vinegar and manske for harmala crystals or b) wash in water to remove base and decant

It would be quick to get a crude extract and not that messy I just wander how much NaOH would be left doing B but if you are very careful with the initial basifying you could keep it to a minimum.
 
geeg30
#16 Posted : 5/26/2015 2:11:15 AM

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NaOH is only really dangerous in sufficient quantities. A few washes removes the dangerous aspect of NaOH. You breathe in more dangerous exhaust fumes every day than what NaoH residues would remain after a few washes.
Here you!!! Gonnaenodaethat

"Iceberg???? - What Iceberg????"
 
ouro
#17 Posted : 6/23/2015 10:01:30 PM

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on review, Dreamer042 and geeg30 both make a good point that you could just collect the preicp after basing the tea, wash with clean water, collect, and be done. I suspect it wouldn't be quite as clean but I've never really experimented and compared. I might try that in a few years when my harmala jar gets low again.
 
ouro
#18 Posted : 11/2/2015 7:35:42 PM

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Update:

After talking to a few people, I think the dominant factor in removing filtering problems is using whole seeds instead of grinding. At this point, there is enough data that shows people getting full yields without grinding seeds, and without too much extra tea brewing, that I strongly advise brewing whole seeds to avoid frustrating filter situations.

By the end of the Sakkadelic extraction thread, a lot of the easy and effective harmala extraction points are layed out pretty clearly. (found here: https://www.dmt-nexus.me...osts&t=66485&p=6 ) Thanks guys!

1) Use whole seeds

-Freeze thawing and using the microwave can make tea brewing less time consuming and more effective. Finding a way to completely drain the whole seeds of tea before starting a new steep also seems to help according to the sakkadelic thread.

2) do not reduce

-reducing is not needed. Simply base the tea and let the harmalas fall out, and discard the waste water. Reducing is a waste of stove time/energy and only encourages impurities to come out of solution and mix with the desired freebase precip.

3) either base before the gunk begins to precip from the tea and discard the dirty waste water, or filter the gunk that precips before basing.

-If you do not reduce and use whole seeds, I'm not totally sure how much gunk is even left in solution that will come out if you wait. It is perfectly efficient and helps the workflow to just base tea immediately after making a steep and discarding the waste water asap after the harmala precips. This also allows the extractor to see the diminishing returns of successive boils to help decide when to stop making more steeps.

at that point you have crude harmala freebase, which can be washed with water, cleaned via A/B iterations, or manske. I suspect it is clean enough after washing with water at this point for most peoples purposes.
 
pitubo
#19 Posted : 11/2/2015 11:54:29 PM

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I'm not sure if it would be good advice to skip Manske salting of rue extract. Do we know reliably how much vasicine, vasicinone and related quinazoline alkaloids are in rue? If substantial amounts of these other alkaloids are present, then the dosage estimates of harmine and harmaline based on extract weight become unreliable.

Also, apart from other medicinal effects, vasicine and vasicinone are uterotonic, meaning they act upon the uterus. Females should be careful about ingesting them.
 
ouro
#20 Posted : 11/3/2015 12:33:02 AM

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By all means manske if you feel compelled to. Honestly I don't know enough about harmala alks generally to give them to a pregnant woman in the first place, regardless of vasicine.

But as far as what we do know:

content of dried plant material for the other alks:

Vasicine (peganine) - 0.25%
Vasicinone - 0.0007%

according to:
Pulpati H, Biradar YS, Rajani M (200Cool. "High-performance thin-layer chromatography densitometric method for the quantification of harmine, harmaline, vasicine, and vasicinone in Peganum harmala". J AOAC Int 91 (5): 1179–85. PMID 18980138.

Plus from personal experience and many other trials reported among rue extractors, basing leftover manske water recovers an extremely small amount of precipitate, which may contain a lot of harmala. I think there was even a lab test of this residue and it was determined to be mostly harmalas, but I might be misremembering. Does anyone recall this? At any rate, the amount of vasicine is very small.

Also note that vasicine is the primary active in Justicia adhatoda. A quick google survey of this plant shows some caution of use during pregnancy, but mostly beneficial effects. I encourage anyone who intends to carry a fetus, or even just anyone at all, to do their own research on these plants and chemicals before ingesting any of them. Personally, I'm not concerned with vasicine content.

EDIT I confirmed with snozz and endless who both tested manske residue and said it was almost entirely harmala alks
 
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