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Syrian Rue Extract to Freebase help needed! Options
 
Jim27
#21 Posted : 2/12/2015 5:20:20 PM
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At this point I'm committed to keep going: 1) because I want it to work 2) I want to verify that it is rue.

Is there a way to finger print the powder?

Last night I dumped 3 grams with a lot of vin. Going to let that sit for a day and then filter out the solids.
 

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pitubo
#22 Posted : 2/12/2015 6:40:48 PM

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Jim27 wrote:
Is there a way to finger print the powder?

Apart from having it analyzed by a modern and well equipped laboratory, not really. What you can do yourself is to hold a UV black light near a solution of the powder. It should glow in a color between green and bluegreen. If there is no glow, there are certainly no harmala alkaloids present. But if it does glow, that does not say how much there is, because harmala alkaloids cause fluorescent glow already at very low concentrations.

Jim27 wrote:
Last night I dumped 3 grams with a lot of vin. Going to let that sit for a day and then filter out the solids.

You should at least try to use lye on your extract. Maybe that works better.
 
thebrownser
#23 Posted : 2/12/2015 6:57:18 PM
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I agree, uv test is a great way to confirm that it is rue.


Harmalas are extremely water soluble in salt form. If the oh is 7 lower they will all get into solution. Adding lots of vinegar just makes it way harder when you go to base, and can lead to excess sodium acetate in the product.

Sodium carb is perfect for this extraction, lye is only ever better in a stb where you are trying to break down the plant material and wash with a non polar solvent. When trying to raise the ph of a solution, lye is no better and is a lot more dangerous.
 
pitubo
#24 Posted : 2/12/2015 7:37:57 PM

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I agree that lye is generally not needed just for basing. Here I suggest using it as a last resort, sort of sledgehammer approach.

Very good point about the danger of lye! Always wear eye protection when working with lye. Gloves are also recommended, both for protection of hands and of glassware. Lye saponifies finger fat, making hands slippery. With gloves, grip is better. Eye protection is most important: lye damages eyes quickly and permanently.
 
Jim27
#25 Posted : 2/12/2015 8:16:46 PM
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I will make the Sodium Carb concentration tonight and mix it with another 5 grams of powder.

- 1/2 Cup Wash and 1 Cup water boiled down... that should do it?

- If it does turn yellow I'll decant into a new jar and let it settle. Hopefully collect my goods

I will also try the black light.

Thanks for your feedback!
 
thebrownser
#26 Posted : 2/12/2015 10:16:18 PM
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Let me go over some basics here to help you better understand, apologies if you already know this.


Alkaloids have two forms
-salt form, formed in reaction to acid, very water soluble.

-freebase form. Formed in reaction to bases, insoluble in water.


Mixing your rue powder with sodium carb and water is going to put the alkaloids in freebase, insoluble form and they will remain in the powder. What you want to do is


Soak rue powder in SLIGHTLY acidic water. Half teaspoon vinegar at most.


Water will turn dark colored and the allalods, along with muddy plant material will be in it.

Let settle and filter as best you can, fridge overnight, decant and filter again. This is to clean the solution from as much plant matter as possible.


Then, add sodium carb saturated solution to the harmala tea, it should poof and go all milky and the alkaloids should snowflake down slowly. Ones settled decant the water away, all the harmalas are the powder on the bottom. Add more neutral or slightly basic water and decant several times to purify the harmalas, and then evaporate the remaining little bit of water.

 
DansMaTete
#27 Posted : 2/12/2015 10:24:53 PM

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Yeah, follow what thebrownser says and don't focus too much on the yellow color. Yellow is what happen when it's quite pure but before the solution can be darker and 'hide' the yellow color.
When you put drop of your basic mix in the seeds soup you should see some precipitation = white clouds forming.

Check pictures(and the tek) here.
« I love the smell of boiling MHRB in the morning »
 
Jim27
#28 Posted : 2/12/2015 10:44:37 PM
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Awesome Brownser!

One question to you method: For the last step I should decant after everything settles.

How long should this take? A day between each wash? Slightly basic water?

"Add more neutral or slightly basic water and decant several times to purify the harmalas, and then evaporate the remaining little bit of water."

You really cleared up for me the fact that I should always work with the tea until the very last step.
 
thebrownser
#29 Posted : 2/13/2015 7:56:15 AM
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It only takes like 20 mins for the alkaloids to settle back down so you can decant again.

And just make sure your tap water isnt naturally acidic when you do your extra washes, because then you will lose a bit of product. Maybe sprinkle a tiny pinch of sodium carb to the water you are going to add, or better yet just buy a gallon of distilled water, couple bucks at a grocery store.
 
DreaMTripper
#30 Posted : 2/13/2015 8:54:51 AM

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Thats the sort of informed and helpful post that will get you a full membership.
 
Bright_Spark
#31 Posted : 2/13/2015 12:02:00 PM

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Hi guys, in a somewhat parallel universe I have been learning the lessons that the kitchen and the plants have to teach me and I must say that my utmost respect goes out to the original pioneers who somehow managed all this stuff in a jungle with dust and dirt and no glass or real temperature control. I have poured away lots of junk, seen all manner of colours and textures in various mixtures and I'm still stumped.

So far the experience is thus :

Followed various teks with mimosa and came up with varying degrees of quite pure and pretty spice.
Vaped in a light bulb pipe - nasty, burning but very swirly twisting visuals for a short while. Not worth the burn.
Smoked with tobacco - much mellowed but still rotten to taste and not the nicest feeling in the lungs. Longer slower visuals.
Smoked with mullein after reading here about it helping reduce harshness - same effect really but not so nasty.

At that point I decided the smoking was not the appropriate roa so I tried 50mg citrate rectally with water via syringe - nada

So I know there's another world there, I've had a glimpse and like it a lot. My problem is some kind of bottleneck.
I can't seem to get past a certain point so I decided to move on to brews that contain everything rather than extractions of things that may or may not be what I want them to be.

To validate the relevance of my post in this thread I have to bring you up to present. The above is my journey so far maybe 8 weeks of practical after months of study and reading.

So on to the seeds. Me and partner first did 3g each crushed rue bombed down in two papers. Followed after 15 by reduced brew from 30g mimosa(determined by to be no less than .8%) She puked and got nothing. I was fine and got nothing. I added some of the spice powder I extracted after an hour and a half - nothing. I start to think my seeds are duff.

In the mean time I had some issue where after I collected some mimosa crystal (stb heptane) freeze precip I had about a gram of yellow goo so I separated it and added ISO then infused the lot on to 1g of mullein. After days of drying I weighed 1.88g so point eight of something in the herb for sure. Upon bioassay it was decided that whatever form of trickery made the crystal wet and goo was not an issue as it was as powerful and same flavour as the crystal alone and actually turned out to be possibly the smoothest test so far.

Next I procured 100g of ourinhos caapi very yellow smelling like reptile tank lining (my head instantly shouts source??? I'm good with smell and wonder could the incidental existence of a kg bag of bark chips in a reptile shop costing 1p per G yield anything interesting?). I made a 15 gram of it and lemon tea French press style and brewed twice and drank. After 40 minutes I smoked .2 of the herb I made previously (assuming ~80mg spice) and I got extended effects similar to before but with an uplifting edge, a feeling of general well being. It was longer lived than any previous smoke and I lost myself in twisting writhing things inside outside every side sort of nowhere for a good half hour. On comeback I chased the place I had been with another two three four joints but never got the same depth and decided this was the effect of the tea that had now wore off.

So here we are and I went old style aya for the next experiment. I procured chaliponga leaf and proceeded to create a brew in the following manner. I weighed 18g mimosa and added to a pot with 20g of chaliponga a tbspn of lemon juice and 500 ml spring water. After placing that one to boil I added 2g of the rue seeds and 50g of caapi ourinhos to a second pot with a tbsp of lemon and another 500ml spring water. I brewed for 45 minutes at low heat then strained the juice to a container before adding another 500ml spring water to each and repeating. I did this three times in total saving the combined boils and straining a few times.
After reducing the final volumes to 10ml for the rue and caapi and 20ml for the spice mix I felt ready and in my head I had two shots to be poured of maoi then four shots of spice tea to be taken after 15 minutes then a spare for a purge or if we wanted more depths upon finding a level. Well. Filthy taste but easy enough to keep down. I had slight tingles from the maoi but maybe placebo. My assistant felt sleepy. We did both shots of the mimonga (my name for mimosa/chaliponga) I had slight visuals and decided to kick start at the one hour thirty mark with a smoke of the herb I made and mentioned previously. Wow.
So I smoked probably .2 and was caught in a detail war where my brain saw more detail and then another part said nope you missed that then I'd see more detail and again nope you missed something else etc. this went on and on with a plant inside the fish tank until I felt myself spasm and went to purge. I felt briefly like me, the vomit and the toilet were falling through space then I was back and washing myself up. This was last nights attempt to learn the secrets. After the toilet I was very mellowed for an hour or so and I chalk this as the most intense journey yet but, here's the big but. I have a deep feeling that this is the tipp of the iceberg and that I'm completely missing something.

I was sure this would be the one. It was not what I was expecting.

So today!

Today I will take the other 30 or so grams of seeds and the 40 or so grams of caapi and I will extract them.
I will share the methods and findings here because I hope that it will add to this thread in the sense that someone may have given up way before now if they had felt the failure as I have. It's not failure. It's the way of things. I fully believe that your experiments with 20x extract are a slow way of these things bringing you close rather than smashing you into another reality.

I feel the only real way to know what's going on is to start with measured doses of the actual active I.e pharma.
The best way to do this is extract the caapi and rue and see what's there and in the process I can determine if I failed by my own hand or if I failed because the plants were not high in active content.
I would like to share a few pictures of various things that may or may not add visual depth to the words I have provided above. I don't seem able to attach them at this point.

Once again thank you everybody who contributes. The information on this post alone will probably be the final piece of the puzzle for me and I will make sure I share everything once I have a proven system in place.
Bright_Spark attached the following image(s):
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pitubo
#32 Posted : 2/13/2015 1:50:14 PM

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The reptile beddings are good. Would you believe that some people apparently want to get ready made harmala extracts for use in a terrarium? Those people must really love their pet reptiles Wink

Anyway, if you don't like the smokes from a glass bulb pipe, make yourself a "machine". Search the forum to learn about it. Another smoking option is changa, a combination of DMT freebase and harmala freebase onto herbs like mullein or damiana.

For the oral route, don't eat whole or ground rue seeds, make a tea instead, or better, a triple boiled and reduced tea, or yet even better - an extract.

Why do you wait time between ingesting caapi/rue brew and ingesting mimosa/chaliponga/DMT brew? IMHO it is just as good or better to ingest the combination at once.
 
Bright_Spark
#33 Posted : 2/13/2015 7:11:20 PM

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Hey pitubo,

I looked at other supplies in the past and did an extract once on a kg of hemp for reptiles to no avail.
I did end up with about a teaspoon of inactive very close in every detectable way for me to vegetable oil. (Was looking for another spice)

I'm not so sure about the machine, It's the actual smoke or the feeling inside me I don't dig.
I used heat from a hot air source rather than fire and it Vaped bud beautifully for that smiley high with warm cheeks with practically no burn or nasty flavour. Of course I could slip some mint and rue extract in to my mystery changa as described above. In fact I did grind and add two leafs of chali and a pinch of caapi but more for texture.(interesting to know harmala is smokeable)

As for the rue to date, I did make a triple boiled tea and described the effects above along with eating the crushed seeds. This was two separate days I was experimenting. Also I drank caapi tea alone and smoked.

Anyway today's experiment went accordingly and I did three separate boils on the 25g of seeds.
I ended up deciding there would be ~2g of alkaloids to recover or there abouts based on 8% I read here.
I also decided a slight deviation from the three boil and discard theory. I did not crush either.

After the third lot of water was removed from the muck I added about 50 ml ipa and I was amazed to find that after a few zaps in my 2.4ghz oven with the spinning glass plate for around 3-5 seconds a go, that something more indeed came out from what I would have thrown away ordinarily.

Do not ask me to explain this but somehow I believe I can see the contents are what I want because there are only two colours, tan (liquid) and dark(seeds) and when I hold it up to my super lab grade kitchen led bulbs I see three colours!
Have a look at the photo it's amazing. I am not smart enough to not jump to two conclusions when I see this. 1 based on someone describing black light reacting with harmala and my knowledge that these LEDs do leak a little uv, that's harmala that's blue/green (who even really knows could be a reaction of anything in the ipa) 2 if I add the ipa extract to the rest and boil it off then whatever that was suspended in the ipa causing the light reaction will now be in along side the three water extracts.

Done. It came to be that all three extracts were joined by the ipa in a single pot and reduced to about 80ml and the lot sits in the fridge now.

I'm not sure weather to filter decant settle etc etc or not as I would hate to think some of the solids are saturated alms but I'm sure in that much water you couldn't saturate with just 2 g of harmala. It's a curve of learning. I will update the results when I have basidfied and extracted it all.

Bright_Spark attached the following image(s):
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Jim27
#34 Posted : 2/14/2015 7:10:55 PM
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I bought a black light and the results are attached.

1 gram - 1 cup of water shaken under a black light.
Jim27 attached the following image(s):
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pitubo
#35 Posted : 2/14/2015 8:49:05 PM

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Jim27 wrote:
I bought a black light and the results are attached.

1 gram - 1 cup of water shaken under a black light.

I don't see any green fluorescence at all? I am sorry to say so, but it looks like you have an extract of something that is not related to syrian rue in any way.
 
pitubo
#36 Posted : 2/14/2015 9:03:09 PM

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Bright_Spark wrote:
I looked at other supplies in the past and did an extract once on a kg of hemp for reptiles to no avail.
I did end up with about a teaspoon of inactive very close in every detectable way for me to vegetable oil. (Was looking for another spice)

It was probably rope hemp you got. Must have been a different reptile supply shop than the one I'm familiar with though, that one doesn't sell any kind of hemp.

Bright_Spark wrote:
I ended up deciding there would be ~2g of alkaloids to recover or there abouts based on 8% I read here.

That is a maximum yield. Don't be disappointed if your seeds and extraction procedure yield less. A 5% yield is quite okay, particularly after purifying.

Bright_Spark wrote:
After the third lot of water was removed from the muck I added about 50 ml ipa and I was amazed to find that after a few zaps in my 2.4ghz oven with the spinning glass plate for around 3-5 seconds a go, that something more indeed came out from what I would have thrown away ordinarily.

If you have a lot of time and very little seed material, you can boil 6 times and still get out a little. It will still glow under blacklight illumination, but there will not be a lot of harmala alkaloids in it. After three good boilings, the yield becomes marginal.

Bright_Spark wrote:
Do not ask me to explain this but somehow I believe I can see the contents are what I want because there are only two colours, tan (liquid) and dark(seeds) and when I hold it up to my super lab grade kitchen led bulbs I see three colours!

Yes, that is harmala fluorescence. The uv in bright sunlight also does it.

Bright_Spark wrote:
Done. It came to be that all three extracts were joined by the ipa in a single pot and reduced to about 80ml and the lot sits in the fridge now.

I wouldn't recommend having any isopropyl alcohol in there when you base the alkaloids, it might make them less prone to precipitate.

 
Jim27
#37 Posted : 2/14/2015 10:07:07 PM
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If the original extraction was done with ethanol would that change any of my findings?
 
thebrownser
#38 Posted : 2/15/2015 12:30:17 AM
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Harmalas love water. Even one seed in a cup of water creates a glow. The florescence is very powerful.


Also I have read but not confirmed that ethanol may react with harmalas, and create something called harmala-red that may or may not still be an active maoi... so I would avoid that.
 
DreaMTripper
#39 Posted : 2/15/2015 12:48:51 AM

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thebrownser wrote:
Harmalas love water. Even one seed in a cup of water creates a glow. The florescence is very powerful.


Also I have read but not confirmed that ethanol may react with harmalas, and create something called harmala-red that may or may not still be an active maoi... so I would avoid that.



I believe burnt did some tests on harmala red and discovered that it was the same as water extracted harmalas.
 
DansMaTete
#40 Posted : 2/15/2015 12:54:40 AM

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thebrownser wrote:
Also I have read but not confirmed that ethanol may react with harmalas, and create something called harmala-red that may or may not still be an active maoi... so I would avoid that.

Harmala-red is harmalas freebase oxydized. It's a dye and ethanol is a solvant for it. I don't think ethanol reacts with harmalas (i could be wrong !)
« I love the smell of boiling MHRB in the morning »
 
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