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Harmalas extraction-syrian rue (by SAKKADELIC) Options
 
ganesh
#21 Posted : 9/14/2015 5:50:34 PM

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Jees wrote:
As promised, I gave some of the ideas here a try


Jees: In your ground seeds tek maybe you should have tried boiling them instead of cold soak? I wonder what yields you'd get with this whole seeds tek if you cold soaked them?

PLUS: I am a great fan of your video tutorials. Could you do one about this? Or better still do one from start to finish with every step, aka 'rue extraction for dummies'?

Love them blue gloves, and sandals. Maybe put a glove on them toes for sake of purity, (must not offend the rue.) Big grin
More imaginative mutterings of nonsense from the old elephant!
 

STS is a community for people interested in growing, preserving and researching botanical species, particularly those with remarkable therapeutic and/or psychoactive properties.
 
Jees
#22 Posted : 9/14/2015 9:41:11 PM

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Thank you.

Quote:
In your ground seeds tek maybe you should have tried boiling them instead of cold soak? I wonder what yields you'd get with this whole seeds tek if you cold soaked them?

I've thought about boiling and/or freeze-thaws on the grind seeds, just never got to it inspired by being contempt with the yield. It might add something.

Cold soaking whole seeds, hmm, doubtful, but we have a standard expression at work when someone comes up with an idea: "Great, now you are going to try this out!" Big grin

I understand it would be neat to have a chart with all possible actions and what their effect is on the outcome. We could give a prize tag on the most important one and a boo-tag for the action that does little. Such chart would be a nice-to-have but takes a lot of comparing works to get to it finally, and then Steven Stokes comes along to tell that his boils are more effective than my boils and we're back at zero. Laughing Or Brenda Bullcock chimes in and tells us to grind even more finer for better etc etc. And perhaps they are right.

BTW one must wear blue gloves, no yellow ones or the yield suffers, and not any sandal works, must be Birkenstock! No sh*t.

* * *

Sakkadelic, yes would be nice to eliminate the overkills. I think center of gravity is the hitting the whole very mushy seeds mechanically strong so their inner content comes out, with whatever means and repeat that. Something like this would be nice:


When watching how apples were pressed juiced, it was important to put them in a cotton bag. I would also do so with the seeds.

Or putting an amount of the seeds in a muslin bag and squeeze it with something like this:


I'm still wondering on the impact of the microwaves, does it more than just heating? I did waved mine shortly to try it (and finding out my oven wasn't good enough, no rotating plate --> heat spots) so I switched to standard boils.

The towel squeeze trick works best for 50 gr seeds at a time so your hands have a good firm grip over the ball of seeds. It's hard to overpower a too big ball like 100 grams in it.
 
Jees
#23 Posted : 9/14/2015 9:55:49 PM

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Also tempting:
Kitchen Pasta Noodle Press Machine Vegetable Fruit Juicer Stainless Steel NIGH
18 dollars at your doorstep Drool

http://www.ebay.com/itm/...9509?hash=item1e8efc9fb5
Jees attached the following image(s):
press.JPG (27kb) downloaded 568 time(s).
 
Jees
#24 Posted : 9/14/2015 10:05:32 PM

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Sakkadelic, did you use this kind of potato masher? Or another kind?


First I thought you used something like this:
 
ganesh
#25 Posted : 9/14/2015 10:25:56 PM

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(with some blue gloves on them feet) Laughing
More imaginative mutterings of nonsense from the old elephant!
 
Sakkadelic
#26 Posted : 9/14/2015 10:31:14 PM

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i don't think the microwave has any impact other than heating it's just faster...
i now know what to buy next Smile thank u jees
this is what i use one jar is usually not enough for all the liquid so i use two then combine after the first basification.
there's no way i can get it right, i tried it straight and it got flipped to the left i tried it flipped to the right and it didn't flip back, only the picture with iphone worked
Sakkadelic attached the following image(s):
20150915_002150.jpg (2,157kb) downloaded 544 time(s).
20150915_002150.jpg (2,173kb) downloaded 543 time(s).
"Is this the end of our adventure? Nothing has an end. We came in search of the secret of immortality, to be like gods, and here we are... mortals, more human than ever. If we have not obtained immortality, at least we have obtained reality. We began in a fairytale and we came to life! But is this life reality? We are images, dreams, photographs. We must not stay here! Prisoners! We shall break the illusion. This is Maya. Goodbye to the holy mountain. Real life awaits us." ~ Alejandro Jodorowsky
 
0100101001100011
#27 Posted : 9/15/2015 1:59:03 AM

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Hi guys,

Just finished a SR extraction with whole seeds. Just wanted to give my feed back.
I ended up with 2.7g of clean extract from 50g of seeds. (5.4% yeild)

My process.

4 x 30min boil of seeds at pH 4.
Collected tea, discarded seeds.

Based tea to pH 12.
Allow to precip in fridge 8hrs.
Carefully decanted 90% of base water, poured remainder with extract via filters.
* This filtering was difficult. Did in 4 batches, replacing filter each time.
Washed extract off filters in acid water - pH 4
Poured acid water with dissolved extract via filter again. Discard filter.
* This filter was a lot easier - one batch slowly.

I then perform these steps again, base/filter/acid/filter.

Then one final base - allowed to precip in fridge overnight.
Then I washed the base 4 times with water to lower pH to 8.
(Decant 90% base water, add fresh water, settle (30min), repeat.

Last step - decanted 90% of water - then pour the rest with extract via filter.
Scraped the wet extract from filter onto ceramic dish.
Allow extract to dry over night then scrape with razor and chop up to fine powder.

I started the process Friday night and Monday morning i was scraping up my ready to consume harmala/harmine extract.

Final product was a light beige powder with a consistency similar to talc, taste test was not bitter - no flavor at all really.
 
Nitegazer
#28 Posted : 9/15/2015 2:52:47 AM

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Sakkadelic wrote:
i don't think the microwave has any impact other than heating it's just faster...


Au contraire mon frere. Microwaving does more than just heat!

Recent Extraction Techniques for Natural Products Paper

from the document: "In the case of extraction, the advantage of microwave heating is the disruption of weak hydrogen bonds promoted by the dipole rotation of the molecules."

and

"Localised heating leads to the expansion and rupture of cell walls and is followed by the liberation of essential oils into the solvent"

I know we're looking for salts here rather than oils, but rupturing the cell walls is certainly what we want to do!

It helps to have a newer microwave that provides a more homogeneous field and a variable inverter to deliver ~600w of power (most microwaves pulse their highest power only).

Since Jayrocco was able to get good results with whole seeds, I'll try an extraction with whole microwaved seeds (after one freeze/thaw). I'll be back with results in about a week!

Thanks Jayrocco for posting results of your experiment!
 
0100101001100011
#29 Posted : 9/15/2015 3:31:02 AM

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You're welcome. I figure if we can spare the mess and the filtering difficulties of having powdered seeds - it would make this process much easier.

The upper yield with Syrian Rue extraction is around 6% with crushed/powdered seeds.
My yield of 5.4% is 80% of a 6% yield. (I believe i may have lost some yield during the first filter fiasco)

So either the acid boils penetrate far enough to get 80%+ of the alkaloids from whole seeds.
OR
80%+ of the alkaloids are in the coating/shell of the seed.

Lets stop with the mess and just use whole seeds!
 
Sakkadelic
#30 Posted : 9/15/2015 6:33:23 AM

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Thank u Nightgazer for correcting me, i hope u get good results too Smile

Jayroco maybe u got less yields because u didn't do enough boils or did u squeeze the seeds?
And did u use normal coffee filters? I find it hard to filter the freebase with coffee filters without loosing product, i think it's better if u just filer the acidic solution..
I find my extract to be a bit bitter maybe there is some impurities left because i don't do filtering i will try to filter as proposed by BongWizard and report back.
"Is this the end of our adventure? Nothing has an end. We came in search of the secret of immortality, to be like gods, and here we are... mortals, more human than ever. If we have not obtained immortality, at least we have obtained reality. We began in a fairytale and we came to life! But is this life reality? We are images, dreams, photographs. We must not stay here! Prisoners! We shall break the illusion. This is Maya. Goodbye to the holy mountain. Real life awaits us." ~ Alejandro Jodorowsky
 
Jees
#31 Posted : 9/15/2015 7:27:30 AM

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Wow Sakkadelic, that wooden plunger seems very rigid stuff Shocked , no wonder you got good results. And that metal mesh seems so fine that it acts like a cotton bag (to put the seeds in). Though I would still favor an extra muslin bag (or a fine cotton sheet) during squeezing.



Sakkadelic wrote:
jayrocco wrote:
... I find it hard to filter the freebase with coffee filters without loosing product,
i think it's better if u just filer the acidic solution...
I agree, there's really no use to filter the very first based liquid. Even more: better to do some A/B transitions before the first filtering of acid liquid takes place, how much A/B's depends on the clear-ness of the liquid showing. Once you have filtered in acid stage, the next filtering of base will be a piece of cake no doubt.

Jayrocco, 5.4% is neat for whole seeds Thumbs up
We must also not forget that % yield is not solely a factor of extraction technique, the potency of used seeds is mandatory, and can vary even greatly. Therefore when comparing workflow/yield one should actually use same batch seeds, something I was able of comparing the grind-workflow vs. squeezed-whole-seeds.


Thus so far we have 3 potent (combined) candidates for success, Sakkadelic tek Pleased
- freeze/thaw, say 2 times;
- microwaves in the process (thx Nitegazer);
- squeezing them seeds hard before re-boiling.
 
Sakkadelic
#32 Posted : 9/15/2015 8:31:26 AM

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I totally agree with everything u said jees there so many new ideas i want to try, i'm waiting for the new batch to arrive i hope it's good quality
Is there anyway we can move this to the harmalas section??
"Is this the end of our adventure? Nothing has an end. We came in search of the secret of immortality, to be like gods, and here we are... mortals, more human than ever. If we have not obtained immortality, at least we have obtained reality. We began in a fairytale and we came to life! But is this life reality? We are images, dreams, photographs. We must not stay here! Prisoners! We shall break the illusion. This is Maya. Goodbye to the holy mountain. Real life awaits us." ~ Alejandro Jodorowsky
 
Jees
#33 Posted : 9/15/2015 10:16:36 AM

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About the microwaves:

Nitegazer hints (thank you!) to the document in attachment.
Can people with lab background interpret this document in relation to our usage here?
Or add info in general about microwaving for our purposes?

What comes to my mind is if the rue seeds have to be totally submerged (boiled) or only moistened (like soaked + strained) for the microwaves to have their cell disrupting effect?

We have this thread: Microwave Assisted Drytek (MAD Tek) microwaving bark in soup consistency, not dry not watery.

And this thread:[Technique] Microwave-Assisted Extraction.
In post #19 someone did rue with minimal water!
BundleflowerPower wrote:
I did a simple experiment with P. Harmala. 12 g was covered with a minimal amount of water which was acidified with 1000 mg of vitamin c. This was microwaved for 1 min.

A freind and I then consumed the rue along with 10 g each of normaly prepared ACRB brew. We drank this over the course of an hour and a half. A very powerful experience resulted.

The tea made from the rue was also very easy to drink compared to the normal 3x boiling method.

I should note that the effects of the rue seemed a little different than normal. More of an electric feel. Perhaps some of the harmalas were reduced to THH in the microwave?

Edit: today I decided to attempt to brew acacia using this method, a sort of bio essay guided research. I covered 5 g of ACRB in a small glass and covered with minimal water. No acidification used. Microwaved for 1 min. I had 140 mg of harmalas which I re-constituted in water and drank, followed 15 min later by the light.

It works. It was almost as powerful as the 6 g rue + 10 g ACRB brew I mentioned above.

Btw, the taste was very tolerable. Better than the egg white trick or letting it decant over and over.

I find 6gr rue overkill, but if he did only what he said then a shallow extraction might have occurred. This might be reflected by the "very easy to drink" remark.

 
Nitegazer
#34 Posted : 9/15/2015 12:30:59 PM

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Good idea putting out the call, Jees, being that I am *not* a trained chemist. Big grin

I do have some basis for how I will proceed, however--- see the attached document that provides some assistance with use of microwave for different solvent/solute combos.

Here are some useful sentences providing guidance:

"increasing the power will generally improve the extraction yield and result in shorter extraction time. On the other hand, high microwave power can cause poor extraction yield because of the degradation of thermally sensitive compounds. Also, rapid rupture of the cell wall takes place at a higher temperature when using higher power, and as a result impurities can also be leached out into the solvent together with the desired solute"

I am not worried about the harmalas being fragile, since the microwave should only heat the solvent to 100c. I don't want to pick up too many impurities, however. The good news here is that a properly tuned microwave may be able to release the harmalas with less impurities, though we won't know til we try.

" In many cases the extraction recovery is improved by the matrix moisture, which acts as a solvent. The moisture in the matrix is heated, evaporated, and generates
292 Fundamentals of Microwave Extraction
internal pressure in the cell, which ruptures the cell to release the solutes, hence improving the extraction yield."


Hence the soaking

"occasionally, when longer extraction time is required, the samples are extracted in multiple steps using consecutive extraction cycles, which are also an example of the use of a larger amount of solvent and higher microwave application time. In this case, the fresh solvent is fed to the residue and the process is repeated to guarantee the exhaustion of the matrix. With this procedure, the extraction yield is enhanced, avoiding long heating."

YAY! BTW, over heating with time seems to present the same problems as too much power, so the issue will be how many impurities will we get with the desired amount of salts.

" in conventional extractions, the use of large volumes of solvent increases the extraction recovery. Studies reported that the extraction solution must not exceed 30–34% (w/v). In many applications a ratio 10:1 (ml/mg) to 20:1 (ml/mg) was found to be optimal"


By using four cycles of 3:1 water:seeds (33% w/v), I have a total 12:1 ratio.


Soooo-- I am open to suggestions, but expect to run each solvent run on high (1200W) for 5 minutes each. See the example given for pectin from grapefruit.
 
Nitegazer
#35 Posted : 9/15/2015 4:56:57 PM

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Bookmark for myself (and for feedback):

One of the problems extracting the harmala acetates from rue is that the vinegar/water solvent is very non-selective, and drags along many undesirables. Harmala acetate is not very soluble in many common solvents (methanol, ethanol, etc). An the alkaloid form is generally not soluble.

So might it make sense to first extract the undesirables from the seeds with a solvent that won't select harmala salts? The amount harmalas lost in the process might be made up for by not having to filter and wash as much. Microwave use may make this initial extraction quick and efficient.

The question is, what is the most non-selective solvent in which harmala salts are insoluble? Ethenol?Or maybe use Basified water for the alkaloid (perhaps at ph10)?
 
pitubo
#36 Posted : 9/15/2015 7:52:58 PM

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I don't have quantitative data, but when I tried 95% ethanol on rue extracted harmala HCl, it appeared that quite a bit did dissolve. Naphtha on the other hand seems to not pick up any amount of harmala HCl.

Once I ground up some rue seeds and did a butane extraction on it, like I used to do with cannabis to make hash oil. I got a golden yellow oil. The seed residue was used in a standard Tao of rue extraction, but it still did not filter easily and several cleanup stages were still required before good looking product was obtained. So it seems like a nice way to get to the seed oils, but not a particularly effective cleanup.
 
ganesh
#37 Posted : 9/15/2015 8:10:32 PM

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Excuse me if i sound rude, but is it possible to keep this tek as simple as possible?

Jees seems to have gotten excellent results with just water and cheap household products; Do we need to make this extra complex/costly for minimal gain, i ask?
More imaginative mutterings of nonsense from the old elephant!
 
pitubo
#38 Posted : 9/15/2015 9:01:09 PM

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ganesh wrote:
Excuse me if i sound rude, but is it possible to keep this tek as simple as possible?

Lol, sure.

1. Put rue seeds in mouth;
2. Chew;
3. Swallow.

Fundamentalist simplificators may even skip step 2.
 
ganesh
#39 Posted : 9/15/2015 9:13:34 PM

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Are you insulting the method, performed by Jees?

A 6% method? ....... ??? Confused
More imaginative mutterings of nonsense from the old elephant!
 
pitubo
#40 Posted : 9/15/2015 9:47:03 PM

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ganesh wrote:
Are you insulting the method, performed by Jees?

I don't think I was insulting Jees?
 
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