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Rue extraction with pressure cooker - Results and Conclusions Options
 
Luuk
#1 Posted : 5/23/2012 12:14:17 PM
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One conclusion from this post is altered - see post further down this page

I've recently extracted 500 grams of rue with a pressure cooker. My idea was to test if it's necessary to grind rue seeds when using a PC. 4 45-minute boils on whole seeds were done, the last one kept separately to see how many harmalas it contains. After every boil I squeezed the water out of the seeds with a dishcloth.



Then all seeds were put in a blender to produce horrible brown goo.



I wanted to test if the 4th PC boil still extracted alkaloids, and if grinding the seeds after 4 PC boils yielded some more.
I tasted all the teas to estimate the amount of harmalas. The first 3 boils were very bitter, the 4th was slightly bitter, but fifth one (with ground seeds) had no bitterness at all.
The idea of filtering this mess for nothing is not very appealing.
To all boils vinegar was added to ensure that all alkaloids are in their (bitter) salt form.


The results are in


After filtering about one third of the pulls through coffee filters I decided that it took way too long and wondered if all the filtering was really necessary. Judge for yourselves!



As you can see there is no color difference between filtered and unfiltered pulls, so all the filtering called for in some teks is really not necessary!

Procedure:

After I basified the pulls for the first time I decanted the brown water, and washed the freebase alkaloids and decanted until the water coming off was clear (like in Gibran's tek). Then I did 1 acidification, filtered through coffee filter, basified for the second time and washed them again until clear water was coming off.

The resulting alkaloids are a light tan color, and pure enough to post the final yield. I'll do a Manske on them later, followed by further purification and (partial) separation into harmine and harmaline.

The first 3 pulls yielded 27 grams, the 4th pull 2,8, the 5th pull (ground seeds) just 1,6 grams, and the coffee filters I cleaned another 1,1 grams. This brings the total yield from 1/2 kilo of rue seeds to 32,5 grams of alkaloids. I have some coffee filters with a lot of alkaloids on them left so yield will be around 35 grams.

A yield of 7%. Not bad! Part of this is of course vascinine etc. and impurities but this is some good rue!



There is something odd about the fifth pull though.
After basification the alkaloids from this pull just wouldn't settle on the bottom of the jar. They aggregated in smaller clumps or something. Does anyone have a hypothesis why this could be? Maybe they are different alkaloids, vascinine and companions? Or proteins? Although proteins would seem unlikely because I acidified and filtered what precipitated after first basification.
This is what the fifth pull looked like (it's the middle one):


Conclusions
-Filtering rue tea, except the initial filtering though a dishcloth, is not necessary.
-When pressure cooking, 3 45-minute boils are enough to get most of the alkaloids out. The same thing probably goes for regular boiling, only then longer boiling times are needed.
-Grinding the seeds is unnecessary.
-Grinding the seeds releases other substances(??)
 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
evil804
#2 Posted : 5/23/2012 1:29:27 PM

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you could base each boil to see how many harmalas precipitate out of solution in each pull, would be a more accurate assessment than tasting.
 
Luuk
#3 Posted : 5/23/2012 1:39:56 PM
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Yeah that was my original plan, and is what I'm gonna do with the first 4 boils. Not sure if I'm gonna filter and base all the ground crap because it doesn't taste bitter at all. But I'll post my yields here when I'm done.
 
tryptographer
#4 Posted : 5/24/2012 8:41:21 PM

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Yeah, that sludge is probably only good for the compost pile if it doesn't even taste bitter.

Good idea about the pressure cooker. Lacking a blender, I also don't want to grind the seeds in my mortar & pestle if the amounts are >3 grams. Even without a pressure cooker it's probably not necessary to grind them if you boil for hours, I just did that with promising yield.

Good luck with that batch!
 
Luuk
#5 Posted : 6/12/2012 11:51:30 PM
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I updated the first post with my results.
 
endlessness
#6 Posted : 6/13/2012 12:27:31 PM

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Thanks for the experiment!

Im curious about a couple of your conclusions.. How can you say that grinding rue is unnecessary if you dont have a grinded control group to compare (or do you? ) ?

When you say filtering is unnecessary, do you mean filtering the solution while the alkaloids are dissolved in it? If so, did you only try with coffee filter? Coffee filter is not effective at filtering rue tea, because there's little surface area, the tea only passes once through it. Its much better using funnel with cotton plug, since there is a larger path the tea passes through the filter, and this cleans more of the coloring substances. Coffee/paper filter is only good when you want to collect what is on top of the filter.
 
Luuk
#7 Posted : 6/13/2012 2:01:33 PM
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Hi endlessness,

It's true I don't have a control experiment with rue seeds ground from the start. However, I performed 4 boils on these seeds unground, then I ground 'em up and performed a 5th (45-minute) PC boil. The tea resulting from this 5th boil on ground seeds didn't taste bitter and just gave a measly 1,6 grams when basified. This lead to my conclusion grinding isn't necessary for getting all (or nearly all) the goodies, at least when pressure cooking.

About the filtering, yes I mean filtering the initial rue tea with alkaloids dissolved in it. Using a cotton plug makes sense, using coffee filters is not recommended. It doesn't filter good and takes way too long.
I don't think I will ever filter the initial rue tea though as it is unnecessary time-consuming. Basifying/decanting the unfiltered rue tea, dissolving the alkaloids in vinegar and thén filtering is very low-effort and leads to these light-tan alkaloids upon second basification.
The Tao of Rue tek calls for lots of filtering through cotton plugs and coffee filters, which is the most time-consuming step in the tek. This experiment shows good results can be obtained with much less effort.
 
damon
#8 Posted : 6/13/2012 2:40:10 PM

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I agree about the filtering, rue and caapi. A lot of junk stays dissolved after basing, so the water washing seems to remove much more than cotton balls. I haven't tried a vacuum setup, but the filtering is such a pain it just isn't worth the effort, especially after reducing and before the first basing. Going through the process twice makes them very clean, a third time I would be concerned about losing harmalas, although without as many tannins they seem to crash out better.

Thanks for sharing!

 
Luuk
#9 Posted : 9/22/2012 2:27:13 PM
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Update - conclusion altered

I extracted some more rue, and did further purifications on my product from the first post.
I don't think my conclusion that initial filtering of the brew is unnecessary was right. It seems I've lost quite a few harmalas due to skipping the initial filtering. They wouldn't settle and I threw a lot away with the water during decanting.

After I combined my harmalas I performed 2 manskes on them to get all the unwanted alkaloids out, and I performed 10+ 'a/b' purifications on them.

I another thread - I don't know which one - endlessness recommends doing more manskes than 'a/b's' for purification because of loss of harmaline. I think this happened to me because when I separated harmine from harmaline at pH 8.7 I was left with 3 grams of harmaline and 77 grams of harmine. This could be because of a defect pH-meter, I will try again soon with a better pH-meter.

I saved the salt water left over after the 2 manske's and basified this. The freebase alkaloids that formed precipitated very very slowly, even after a couple of purifications. They behave the same as the alkaloids I got from my fifth pull (see first post). Maybe vasicine/deoxyvasicine/vasicinone precipitate in smaller crystal formations than harmine/harmaline? Just a hypothesis.

Anyway, this is what the alkaloids from the basified manske water look like, followed by some of my harmine (left) and my harmaline (right).
My final yield was 4.65% (with manske water alkaloids) or 4% (without manske water alkaloids).
Luuk attached the following image(s):
2012-09-22-698.jpg (1,784kb) downloaded 446 time(s).
2012-09-22-700.jpg (1,219kb) downloaded 446 time(s).
 
Luuk
#10 Posted : 9/26/2012 4:38:06 PM
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Dagger wrote:
Quote:
They aggregated in smaller clumps or something. Does anyone have a hypothesis why this could be?

I have experienced that on occasions. I think that is because you have a lower concentration of alkaloids. Makes it harder to get it to settle. Since there isn't much other crap in there, it should be relatively easy to filter.

I don't think it's that, because when I dissolve manske'd harmalas (so only harmine/harmaline), and basify the solution they crash out in large clumps and settle fast, even at very low concentrations. It could be an impurity? Is the crystal structure of vasicine/deoxyvasicine/vasicinone known?

Dagger wrote:

Rue seeds can easily be extracted whole without a pressure cooker. Cook for 10-15 minutes, and pour through a fine mesh strainer. Then back on the plate again. Repeat until there is no more bitterness left.


Yeah filtering ground P. harmala seeds is a pain in the ass, and with a pressure cooker really not necessary.
 
boogerz
#11 Posted : 10/22/2012 11:23:11 PM

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Interesting post- I got similar results as your fifth boil after blending my exausted whole rue. Thanks for sharing!
 
 
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