Extracting from "10x Rue Extract"

[merkin]

I have been considering this as a way to save shipping costs. While product in seeds is relatively inexpensive shipping to where I am is most definitely not, often 3-4x the cost of rue seeds. But searching here I see many comments like "people have had problems" etc but no definitive comments about it or its fitness for further extraction to get to the Harmalas (as opposed to direct consumption).

Is it possible? Surely if the extract can be eaten it contains the alkaloids? Also its described as an "ethanolic" extraction. What exactly is this stuff in relation to seeds and the usual extraction teks which start with boiling?

Can you boil this and then base it? Does anyone have any idea or direct experience with this? Its really cheap so getting two kilos is less than 30bux, but shipping a LOT more.

In description on one site: "0.2g to 0.3g contains enough harmine and harmaline to block MAO activity for about six hours" - - seems to imply it contains the necessary alks?

So - can one feasibly and effectively extract Harmine/DHH from an "ethanolic extract" 10x of Rue?

Thanks

 

[Elrik]

Lets consider what is in the seeds. They have protein, various sugars and carbohydrates, fixed and volatile oils, and organic salts of the alkaloids.
Industrially [roughly speaking], the seeds are ground, shoved into a pipe, and hot ethanol is forced through the pipe until it comes out colorless. The ethanol 'tea' is then filtered and the ethanol is distilled off to be reused, leaving the "10X extract" behind. That is the most likely method.
The resulting hardened taffy-like extract would be a mixture of alcohol soluble sugars, other small organics like coloring matter and acids, fixed oils, any volatile oils that didn't co-distill with the alcohol, and organic salts of the alkaloids.
I can imagine the difficulties people vaguely mention. They're trying to get a fat filled dried taffy to dissolve in water [hallucinogenic rock candy :shock: too bad it tastes like harmalas]. If I was trying to refine it first I would break it up into sand or powder [wear gloves, as the powder would stick to the moisture in your skin] and then I would apply one of two simple approaches, either I would try to initially dissolve it in a warm alcohol-water mixture to help the fat move around, or I would be patient and simmer it in slightly vinegar acidified water with stirring for a good long time to get the fat to melt while the sugars and alkaloid slowly dissolve from it. Just dumping all the crushed extract in would make it immediately harden into one chunk again, so cast a spoonful of crushed extract in and stir, repeat as appropriate.
I would probably choose option 2: smash it up and simmer for hours in mildly acid water, replacing any water that boils off before it is dissolved. I'd then let it cool to only mildly scalding, filter it through a coffee filter, probably boil again to remove much of the excess water, dissolve in 15 grams of rock salt for each remaining 100ml while still scalding, let cool, refrigerate for a day, collect the manske crystals.
It could also be based, if you go that route remember not to add base to hot water.

I wonder what they do with the essential oil byproduct. I love the coffee-grounds like smell of harmala seed.

 

[merkin]

The resulting hardened taffy-like extract would be a mixture of alcohol soluble sugars, other small organics like coloring matter and acids, fixed oils, any volatile oils that didn't co-distill with the alcohol, and organic salts of the alkaloids.

Thanks. They all seem to be offering this as a brown coloured powder so it seems they have dried that 'taffy' or whatever residue they got. I have seen Caapi extracts as a resin though, but this is definitely rue. I suspect you are spot on about their method.

I would probably choose option 2: smash it up and simmer for hours in mildly acid water, replacing any water that boils off before it is dissolved. I'd then let it cool to only mildly scalding, filter it through a coffee filter, probably boil again to remove much of the excess water, dissolve in 15 grams of rock salt for each remaining 100ml while still scalding, let cool, refrigerate for a day, collect the manske crystals.

I think that essentially I take from your response that the alkaloids are actually in there somewhere and it is then the challenge to get to the point where it dovetails into the standard 'seed' tek. I was thinking to try and dissolve in water - if not, try vinegar water. If it dissolves in that then boiling and manske I'd imagine is the next best step as you said.

Essentially treat the powder as a form of ground seeds? Anyway, at the price its certainly worth a try as the shipping cost is a 0.1x advantage over the seeds.

 

[monomind]

A while ago I got some rue extract in powder form. It was cheap and I thought it might be an easier starting point for an extraction rather than working with seed.
I tried to acidify, to manske, to basify... but nothing happened.
No alks in any form precipitated.

 

[Kumarajiva]

A while ago I got some rue extract in powder form. It was cheap and I thought it might be an easier starting point for an extraction rather than working with seed.
I tried to acidify, to manske, to basify... but nothing happened.
No alks in any form precipitated.

It was not rue extract then. Probably some other maoi sold as rue with some filler.
If its true rue extract its ok to use it as starting material.

Ethanolic extraction will be heavily contaminated with oils though.
I used to do ethanolic extraction with soxhlet and had to distill the alcohol (adding water in the middle of distillation)
and was left with two distinct fractions of oils floating on top and alkaloids dissolved in water below, and then separate it.

 

[Elrik]

That is a good point. It certainly is possible that some or all harmala extracts are MAOI adulterated fillers.
Like the cheapest off-spec instant coffee available + pharmaceuticals.
This kind of thing happens more than one might think. Remember the marijuana alternative 'Spice' that was sold years ago, it said it was natural herbs but it was synthetic cannabinoids.
Many mainstream bodybuilding supplements, over the years, have been found to contain pharmaceutical drugs or analogs.
Much of the ecstasy or RCs sold contain little or none of the claimed drug. Heroin that's nothing but fentanyl, etc.

If you try this, start with a smaller order and don't trust it until you see a solution glow vibrant green under blacklight and crystallize from a salted solution.
Then, based on the yield you can decide if it is a source that can be scaled up to provide all you need.

 

[merkin]

Thanks for all the input. I have ordered a 'free sample' (1 kg!!) just had to pay the shipping of around forty odd bux. Hopefully it works (a lot) better than monomind's extract!

 

[merkin]

OK. I finally got hold of this extract powder and would like to see If I can get something out of it. It is labelled "Peganum Harmala Extract" and they say via solvent extraction (ethanolic?).

It is a light brown color, much like slightly cleaned full spectrum, very fine and dissolves relatively easily in warm water and also slightly ~pH3 vinegar/water.

I took 5g of it and dissolved in 300ml vinegar/water mix and it turns the familiar red brown color.

First took half of the liquid, diluted again to 300ml with dH2O. Dropped in some KOH solution until pH hit over 10 while stirring. Nothing precipitated at all. Added more KOH solution but it remained same color and translucent. No clouds no nothing. Very slight flourescence.

Took other half, added dH2O up to 300ml (pH3,8 ) and heated to ~90°C and added to same volume 80°C sat salt solution. That is slowly cooling right now.

Any pointers as to what to do or try - given that the goal would be to get to extracting a harmala FB or HCl mix I can later separate? Basically to have this at some point become a known step in the regular extraction tek process - using this 'extract' rather than starting with rue seeds. Since I have a kilo of it theres room for experimentation here.

Thanks

 

[downwardsfromzero]

Very slight flourescence.

Unfortunately, I'd consider that a bad sign considering anything more than the slightest trace of betacarbolines (well, in this case principally harmaline, I guess) produces a quite noticeable fluorescence.

It seems fair to say that Syrian Rue extract does not necessarily equate to betacarbolines. A clear indication of the solvent used would be useful, as would the actual plant parts used. Making the assumption it's from the seeds is just that, even if it's pretty safe to do so. It's still better to be sure.

You might have to basify that whole kilo to stand a chance of recovering anything. It's smelling a bit like a scam at the moment, but I hope the Manske attempt works out better for you.

 

[starway7]

what about the common belief that all of rues actives are on the outside of the seed casings?

And the white inside of the seed is not wanted?

Could there be something on the inner white part of seed that is needed?


I did a simple extraction of outer material on the rue seed using grain alcohol....here are photos below... is not this the rue actives?

 

[downwardsfromzero]

what about the common belief that all of rues actives are on the outside of the seed casings?

And the white inside of the seed is not wanted?

Could there be something on the inner white part of seed that is needed?


I did a simple extraction of outer material on the rue seed using grain alcohol....here are photos below... is not this the rue actives?

Well, clearly it's the rue actives. And we can see that you've made an extract from whole rue seeds.

Imagine this - you do a couple more soaks on those rue seeds. Another soak would have but the faintest fluorescence, but you don't do that. Instead, you grind up the seeds, boil them in a few changes of water and then evaporated the painstakingly filtered aqueous extract. Then you'd have a very slightly fluorescent rue extract that is, in all likelihood, of little use as a source of harmala alkaloids. And you wouldn't be lying if you described it as "Syrian rue extract" either, but without any further explanation it is at least disingenuous to do so.

The inner part of the seed will contain fats, protein and starch but I can't comment on what secondary metabolites might be present without having to look it up.

 

[merkin]

Yeah it would seem you’re right about this downwardsfromzero.
Manske gave no result. Saturated some more, nothing. Serious basing of dissolved powder in hot water with KOH, absolutely no milkyness. Would seem pretty hopeless to expect to get anything out of this.

 

[Burnttoast22]

Sorry for resurrecting a old thread but im having an issue with my Rue extraction and figured I'd ask here instead of creating a new thread.

I acquired some 'full spectrum rue extract x5' and decided to follow the GordoTek for extracting Harmalas.

My issue started when it says in the instructions to follow the steps from 40:25 (video timestamp) if you already have full spectrum extract.

This is halfway through a step. Just before you're supposed to add hot vinegar to the dry powdered alks and let it sit for 6 hours and then filter and keep the liquid.

The video continues from 40:25 to make up a hot salt solution with 1g of salt per gram of dried alkaloids and 4ml of water for evry gram of salt and then combine both hot liquids.

I did this but then wasnt sure what to do with the powdered alkaloids as I wasnt sure if I should just dissolve them in hot water or dissolve them in hot vinegar.

I decided to dissolve the alks in hot vinegar and then add the hot salt solution and stick it in a cooler with boiling water for 8 hours for the crystals to precipitate out.

I did this but nothing precipitated.

Thinking I had ballsed it all up I figured it would be worth trying to at least get the alks back and try again.

So , I basified the alk/salt solution to 9.6 and sure enough the liquid went a light tan colour and solids started precipitating out.

Ive now filtered this and have the powder drying in an oven. So, hopefully I am back to where I started with some dry alk powder.

My issue is I dont know what to do next. Should I re do the hot vinegar step, let sit for 6 hours and filter like I did last time or simply add hot water to the alks and do some manske steps like the tek says.

TBH I was gonna just try hot water and salt this time but thought it might be worth asking if anyone has any experience of this? im pretty sure what I bought is for real as it fluoresce's under UV light and Ive definitely got something to precipitate out at 9.6ph.

 

[Burnttoast22]

OK, so whatever I precipitated from the rebased liquid weighs about 2g's. It kinda looks like it did when I first bought it but just a lot less.

This seems to be in line with the yield you would expect from 25g raw extract but Ive not been through any of the purfying steps yet.

Im gussing either I wasted a lot in the initial acid/salt soak or it was crappy alk's to begin with.

Should I go ahead with the manske purifying steps now or is a waste of time with that little material?

 

[Burnttoast22]

Just wondering if I used the wrong type of salt. I have dead sea salt which is apparently sans anti-caking agents but on reading the ingredients it says it is ionized or at least has ions in it.

Ive ordered some natural rock salt which is supposed to be 100% no additives.

 

[downwardsfromzero]

Ions are an essential characteristic of any salt. "100% no additives" does not necessarily equate with purity though. Dead Sea salt typically contains loads of magnesium and other ions besides sodium and chloride. Kosher white rock salt is about your best bet - that should be about 99.99% sodium chloride.

 

[Burnttoast22]

Thanks for the reply downwards I'll pick up some kosher salt then.

Do you have any thoughts on how I continue the extraction? I have 2g of material that precipitated out at 9.6ph. I just dont know what to do next. If I understand the tek corectly now is the time to acidify it with vinegar, filter and then do the first manske purifying step.

This is exactly what I did the first time on all the material (25g) but nothing crystalised out.

Im beginning to think I just need to buy some rue seeds and do a full extraction (probably using the EA approach)

 

[merkin]

Your extract is still a little dark but its nevertheless close to what it should be. Maybe try a couple of rounds of base-acid-base-acid... (no need to watch pH as just eyeball it - high ph=precip, low ph=solids dissolve) - with a filter while in the acid phase to 'clean' it a bit before you do the Manske - towards a more tan color rather than dark brown? The cleaner it is the more golden clear the color of the acidified liquid (as opposed to deep red/opaque).

Each step loses some product, but a full spectrum extract shouldn't be that dark ime. Your first Manske can be tricky (or not). Cleaning rue extracts feels like a never ending process sometimes! When you filter the acidified liquid there always seems to be some black stuff in the filter no matter how many times you do it. A manske done on a 'dirty' (dark brown) powder usually produces long and spiky, dark red crystals, while as it cleans they become more golden clusters (looking a bit like sparkling like banana slices).

Also the Manske is not strictly necessary unless you are worried about those extra alkaloids that apparently play havoc with pregnancies. If that is an issue though, then definitely do the Manske.

What is your goal here? Full spectrum freebase? Full spectrum HCl? Harmine/DHH separated?

 

[Burnttoast22]

Hi Merkin, thank you so much for replying.

My end goal is to have somewhat pure Harmaline/Harmine and then convert some of that to THH. That way I can dose DMT + Harmaline/Harmine + THH at the correct level.

I originally acquired 50g of alledgedly x5 extract. According to the GordoTek you can skip everything up to 40:25 in the vid.

I acidified the first 25g, left it to sit for 6 hours and then did a manske. result I got nothing.

I then basified the liquid and got 2g of preciptate out.

The second 25g I went straight to the manske step and also got nothing.

I have just basfied the second batch, filtered and the powder is now drying.

Hopefully I will have 4 or 5g total to do whatever it is I need to do next.
----------------------------------

I will do another A/B on it and then go to manske. Im gonna acquire some more rue seeds and use the EA approach as Im not gonna have enough to make any THH this time I think.

My main question is:

When I do the first Manske step, the tek says I need to make an acidic powder solution and then add the hot salt saturated solution to it and let it cool slowly overnight to get the first set of crystals.

This was the first thing I tried and I got nothing.

I just want to check that this is the next step as in the tek the 2nd-5th manske you just use hot water for the crystals and dont add any acid just more salt.

Sorry if im being dim, I have a very good working knowledge of DMT and Mesc extractions I just dont know why hes acidifying it again before the manske as if I understand the process correctly this would stop anything precipitating out.

Thank you for taking the time to give me a hand with this :thumb_up:

 

[doubledog]

I would recommend to start any rue seeds or rue "extract" extraction with precipitation from basic solution. You can see whether you have some alks there (or not) almost immediately.