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Kash's Advanced LSA Extraction Options
 
vixintrex
#101 Posted : 9/2/2022 3:38:11 AM

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Kash wrote:
In response to a few pm's about subbing in materials... This procedure is the way SWIM has used with success and had zero problems every time. The materials can be procured EASILY without any specials licenses or access by anyone, and if you want a smooth extraction, use the materials mentioned.

That being said, SWIM beleives it would be possible to sub in some materials if people want to do so at their own RISK as I have not tried these...

Can recommend substituting ammonia and naptha. Ammonia can be possibly subbed with a decently concentrated sodium bicarb solution or a very carefully made light NaOH (Lye) or KOH solution, each requiring a pH of 9-9.5. If pH gets too high it will destroy the lsa, too low it wont extract. The naptha can be subbed with just about any organic solvent not miscible with H2O.

Tartaric acid could likely be subbed with fumaric acid.

As for the dcm/toluene, SWIM would really recommend just going to the small local hardware store and buying for 10$ in the solvent section... Other things may not extract as well and cause an emulsion. SWIM doesnt like Xylene smells horribly.


hey when you say ammonia do you mean like cryogenic liquid ammonia or like ammonium hydroxide?
 

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vixintrex
#102 Posted : 9/2/2022 3:46:02 AM

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Kash wrote:
Orion wrote:
I'm curious how this would turn out using sodium bicarbonate instead of ammonia. It's more commonly available much less likely to drive the PH up too high.

Is this thread worth a sticky maybe ?


Someone is going to be diving back into this soon, but if I remember right Sodium Bicarb PH is not high enough to push LSA into freebase form.

Ammonia is available in hardware cleaning sections without additives, as well as internet market now days. It will usually go by some other product name however.


so ammonium hydroxide
 
Ruffles
#103 Posted : 5/1/2023 1:02:14 AM
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Trying to revive this if anyone is still out there...

first off... thank you Kash. Second off... thank you Nexian comrades.

Here is a question: For the first solvent step - step 2 = extraction using anhydrous acetone in powdered seeds - why use straight acetone instead of a pinch of citric or fumaric or tartaric in the acetone??? Why not decrease pH at this step to help with extraction like it is done in the equivalent first steps of DMT extraction?
To try to answer myself: Fumaric, tartaric and citric LSA has too low or no solubility in acetone at room temp, therefore `natural` salt of LSA (a natural form soluble in acetone whatever it is - tannic?) would be preferred for it to jump into acetone, plus freebase LSA is also soluble. Please comment here if anyone is better informed. Or we are expecting LSA in seeds to be in freebase form?

Another question: At which step the blue fluor of LSA pops out under UV? Seeds don`t seem to have any blue and the green fluor in the 2nd step doesn`t look like LSA at all.

An observation:
- The green product of step 2 extraction while in the freezer heavily precipitates white clouds, certainly it isn`t all LSA in any form. Very likely to be fats and salts, obviously I am not sure at this point and will investigate further. However, I liked this because wherever LSA is at this point, it may be a separation process step.
 
Twilight Person
#104 Posted : 5/1/2023 8:39:48 PM

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Quote:
Why not decrease pH at this step to help with extraction like it is done in the equivalent first steps of DMT extraction?


Well also not sure but just a general thing is that if molecules get bigger, then they are less likely to exhibit a true ionic behaviour. For example NaCl salt is really small and has a high density of charges. But if you have a pretty big LSA molecule just 1 charge will not count in so heavily. Because of that bigger molecules in general have a better solubility in non-polar solvents when having the same amount of charges.

Of course for bigger molecules they could also contain more Nitrogen which can get also charged via H+. But then again chance for multiple charges is decreasing more and more as it is not favored energetically. That's also a reason why citric acid has a different pKa for every of its 3x H+, making it less likely to detach for every other H+ that has already detached / been deprotonated and thus reducing acidity for every next deprotonation step.

As also the anion of those LSA will be big (and not like Cl-) it's quite likely that those salts just have a good solubility in acetone in general.

Now not sure if that was the initial thought, I guess it was more empirically tested and seemed fine. But that could be an explanation?

A reason to not directly use pH 3 water for extraction might be that this catches up all Alkaloids, while Aceton will only dissolve the big ones and not small ones, where aceton would be too unpolar?


Quote:
Another question: At which step the blue fluor of LSA pops out under UV? Seeds don`t seem to have any blue and the green fluor in the 2nd step doesn`t look like LSA at all.


Sadly I dont get what step this is in the TEK. Step 2 at first page tells to just use seed powder in acetone for initial extraction? In general any extract should have some fluorescence as it would not matter if you mix non-fluorescenting and fluorescenting substances, as long as some are fluorescent they will always give a glow in black light. And as you hopefully carry some Ergot alkaloids right from the first step over into your liquids, they should always glow.


Also when now reading that TEK:

Quote:
8]Quickly add 50 ml toluene or DCM to the solution and mix well for 15-20 minutes.


Mixing 15-20 minutes seems pretty overkill. As this step is not concerning exxtraction from a complex matrix like crushed seeds but instead just regular liquid-liquid you would be done in 2 minutes with hand shaking or even 30 seconds if you could use a magnetic stirrer at 500 RPM+.

Ethyl Acetate would be a good solvent which evaporates speed-wise inbetween and is completely non-toxic. Also no adduct-formation like with DCM, but probably it evaporates so fast that adduct formation is not a thing. Still evaporating Ethyl Acetate with a fan will make you get some water into your product, so you would need a drying agent to calculate your yield.







PS:

At this moment I really need to point out how crazy it is that this guy still is a new member since 2008 and still has made 1200 posts Laughing Laughing Laughing But how is he even allowed to post here, as this is not open for 'new members'?
~ O ~
 
Loveall
#105 Posted : 5/2/2023 12:15:26 AM

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Before the nursery was implemented people could post anywhere immediately after making an account. Also, post nursery it is still possible to demote full members.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
Ruffles
#106 Posted : 5/2/2023 12:49:51 AM
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Hellow Twilight.

So you are saying this extraction from seed pulp with acetone by itself grabs LSA as well as possible and adding acid doesn't increase solubility of it in acetone anyways? But adding it would grab more junk?

Quote:
Sadly I dont get what step this is in the TEK. Step 2 at first page tells to just use seed powder in acetone for initial extraction? In general any extract should have some fluorescence as it would not matter if you mix non-fluorescenting and fluorescenting substances, as long as some are fluorescent they will always give a glow in black light. And as you hopefully carry some Ergot alkaloids right from the first step over into your liquids, they should always glow.


They might give always give a glow but other things might quench its fluorescence. Also, other abundant or more efficient pigments or fluorescent things might catch the UV and prevent it from exciting LSA. And the other things might catch that LSA blue glow for them. Then we won't see the LSA blue glow.

Experimental data here to answer my own question: very clear blue glow shows up starting at step 6 - defatting. Aqueous acidic fraction turns greenish blue (another fluorophere giving yellow? Yellow plus blue equals green), then after a couple of washs with nonpolar the aqueous fraction, gets clear blue. After basification (step 7) it remains clear blue. At step 8 - nonpolar pull - blue glow jumps to nonpolar fraction, succeeding 2 pulls continued to get blue. Heating up mixture of polar-nonpolar to 42 Celsius during pull makes the blue nonpolar a bit more greenish (pulling the yellow fluorophore?), certainly stronger fluor so probably pulling more. Also, it proves an obvious point: it glows blue whether freebase or salt.

Using a very simple UV light like the one used to check bills works very well for this. It is a pretty good way to track where LSA is assuming the blue glow is strictly from it at the point it becomes obvious. Pretty helpful during phase separation.

Anyone has fluorescence spectra for LSA and other ergotamines??
 
Twilight Person
#107 Posted : 5/2/2023 6:33:31 PM

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I'm quite convinced that LSA + it's counter ion is so big that they will exhibit less of 'classic salt' behaviour and thus be more soluble in a semi-polar liquid like Aceton. But of course I have 0 experimental data for this and I even think Kash has no analytic proof, I guess this extraction was more like an empiric process? So as long as it seems to indeed catch it up, I would go this way because the pH 3 water method could indeed catch up more stuff.

THX for the fluorescence explanation and indeed that sounds like a good way to keep track. Indeed many things change it's colour based on being freebase or salt (like pH indicators), but seems for LSA it's not the case. It does not have many double bonds apart from the original indol ring at the bottom. So I would not expect any absorption past 350 nm. Fluorescence emission might be then around 390 - 450 nm which will make it glow blue.
~ O ~
 
Ruffles
#108 Posted : 5/2/2023 10:34:39 PM
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Kash could explain his reasoning on the switch on acetone before defatting.

Yes, harmalas switch fluorescence on and off like that. LSA's blue seems to be quite weak, as it is easily occluded by the junk... Also perhaps the blue emission may be more excitable absorbable to by other molecules.

I am very curious about the green fluor... It might be anything causing it of course... LsA itself might form excimers, which are fluorophores that shift their emissions when in high concentrations so maybe the green happens when it's concentrated (green is just below blue in spectra so it's kind of backwards, excimers usually give higher energy emissions)?? If so this would help assessing how much is in there. Just speculation though.
 
igorcarajo
#109 Posted : 5/5/2023 12:35:42 AM
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I have two questions:

1) Kash says that the product is LSA. Has this been verified by anybody?

2) Does anybody have dosage ranges based on mg of the final product as opposed to the number of seeds used?
 
_Trip_
#110 Posted : 5/5/2023 1:36:25 AM

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I don't think there's been any formal LC MS testing.

Dose wise Albert Hofmann I think took 500mcg IM and noted only threshold effects. I think it's generally thought to be one tenth to one twentieth as strong as LSD. Meaning 1 tab equivalent in LSD would be approx 1-2mg of LSA. (If LSA is in citrate form this dose would be higher again). IIRC I think Loveall in a previous posted noted a paper that stated 6mg was a normal dose.

There's also a big difference in trip reports when comparing HBWR to MG. This is something that needs further investigation as there is likely a difference in the profile of actives between the two (especially fresh MG which may contain more LSH). Although this is not confirmed.
Disclaimer: All my posts are of total fiction.
 
igorcarajo
#111 Posted : 5/5/2023 2:17:24 AM
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_Trip_ wrote:
I don't think there's been any formal LC MS testing.

Dose wise Albert Hofmann I think took 500mcg IM and noted only threshold effects. I think it's generally thought to be one tenth to one twentieth as strong as LSD. Meaning 1 tab equivalent in LSD would be approx 1-2mg of LSA. (If LSA is in citrate form this dose would be higher again). IIRC I think Loveall in a previous posted noted a paper that stated 6mg was a normal dose.

There's also a big difference in trip reports when comparing HBWR to MG. This is something that needs further investigation as there is likely a difference in the profile of actives between the two (especially fresh MG which may contain more LSH). Although this is not confirmed.

Thanks for the reply. So this tek is useful for extracting from either HBWR or MG? Also, which of the two seeds contains more β€œactives”, by weight?
 
_Trip_
#112 Posted : 5/5/2023 2:26:24 AM

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HbWR is way better by weight but fresh MG should contain more LSH (which degrades to LSA I believe hence the difference in trip reports).

IIRC, HBWR for a trip requires only a few seeds, MG is hundreds.
Disclaimer: All my posts are of total fiction.
 
igorcarajo
#113 Posted : 5/5/2023 4:13:05 AM
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_Trip_ wrote:
I don't think there's been any formal LC MS testing.

Thanks. The reason why I asked is that I saw in a white paper that HBWR seeds were found to have 0.3% of total alkaloids by weight, but LSA accounted for only 1/8 of the total alkaloids. So I’m curious, how is it that this tek supposedly only extracts the LSA and leaves behind all the other alkaloids.
 
_Trip_
#114 Posted : 5/6/2023 1:47:25 AM

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Certain compounds can be selectively crashed out of solvents etc with certain acids (salts). The cielo tek is a good example of this with mescaline. But as mentioned no formal testing as far as I'm aware for Kash's LSA tek.
Disclaimer: All my posts are of total fiction.
 
Ruffles
#115 Posted : 5/15/2023 1:09:29 AM
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Hello all.

Here is a contribution to the tek:

After acetone xtraction and filtration, put it in the freezer, let the clouds of fat form and settle. Collect acetone avoiding fats quickly while acetone is cold (Ice bath helps, fast pipetting too) and set it aside for drying or reuse it into mush to load more LSA into it, followed by more freezing and separation. This reduces fats in the initial acetone extract considerably and speeds up washing and basification by reducing emulsions.

Fat Clouds seem to completely lack fluorescence which stays in cold acetone. Emulsion is a major hindrance without some serious defatting. as it is, it takes too much nonpolar solvent on the acid washes, it's a waste. After freeze defatting everything else flows far better.
 
Brennendes Wasser
#116 Posted : 5/15/2023 11:36:53 PM

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Quote:
put it in the freezer, let the clouds of fat form and settle


That's indeed true. I ran that also some time ago, but the product got lost on the way Sad(

Wanted to get some pure LSA as a solid, but as prices for these seeds have gone up so much in the last 5 years you can now only buy 100 seeds instead of 100 g. As definite LSA (not other inactive ergotamines) content seems to be not much higher than 0,1 % obtaining some pure LSA seems a hassle, especially as the TEK calls 50+ seeds equivalent strong, even though if that would be eaten it would rather feel like an intoxication Twisted Evil



Here is just a summary of also some pictures.

First picture is the stuff directly derived from the Acetone extraction. Mostly yellow stuff, I think it was quite a lot, but therefore only traces of active components inside there. And this stuff indeed was not easy to dissolve again in room temperature Acetone, so a freezing step may get rid of a lot of this prior to extraction.

Next step would be collecting all the Alkaloids with pH ~ 3 Tartaric Acid (aq). But at this step you mostly leave the fat layer intact. Then I was afraid I might loose too much LSA still inside this big layer of beige fats.

Therefore another tweak could be adding pH 3 tartaric acid (aq) AND ALSO heptane. This did not dissolve the fat, but made it release from the glas. Then I could shake the flask quite well and hopefully break up more of the fat layer to take up more of the LSA potentially hiding inside.

Also attached is the TLC of the crude Aceton product. A blue fluorescence spot at the top and a green one below. The beige fats will form a pretty big line all along the TLC (Methanol + 1 % Ammonia). As LSA is reported to be blue it would rather be the upper spot, but it is running surprisingly upwards. Would have expected it to run more at the spot of the green substance?

Anyways later when doing the defat the Heptane got the green fluorescence and the water stayed blue. So like Ruffles told the green one seems not what we are after. Here I indeed had some emulsions with all those fats. They did not even get removed pretty well by the Heptane and I had to cut off a sacrificial layer between both phases. In cases like this with DMT Toluene pretty nicely destroyed any emulsion for me, but I think a more polar solvent has a higher chance of also dissolving LSA salts, as big salts tend to migrate more into NPS than small ones.

Then the last step failed for me: Basify to pH 9,5 - 10,0 and extract with solvent of choice (DCM). I used a freshly calibrated pH electrode and still got a colour change at pH 9,6 from yellow to green-blue. Then extracted what should now be freebase LSA, but my NPS stayed completely white, while the water stayed blue. Just out of fun I basified to 10+ and extracted with DCM and also Toluene. The colour never made it into the NPS ... Evaporation of NPS yielded 0 product.

So maybe it got lost on the way or I just had too less seeds, if the alkaloid content really is that low. Did not grant me anything at the end, but maybe pictures can be a reference.




A question which still arose back then:

It was told to not overshoot on pH as at > 10 it would induce creation if Iso-LSA. But I read in a paper they found even more Iso-LSA than LSA already in the plant. Probably would not favor the creation of even more Iso-LSA, but both are Diastereomers (only 1 out of 2 chiral site is changed) and so one could be sterically favored. But as I see it it should be the regular LSA as the Amide is in Cis position to a Hydrogen (small residue). Maybe then this problem would only arise when you already start with a pure Lysergamide, like what you would have on a LSD Blotter?

In any way still it seems at this step it screwed things up for me and then did not want to buy more seeds Sad
Brennendes Wasser attached the following image(s):
Picture L.png (769kb) downloaded 68 time(s).
 
Ruffles
#117 Posted : 5/17/2023 2:25:46 AM
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Great work Mr. Wasser!

Considered doing a nonpolar wash to get some fat out as a first step before acetone extraction. But like you indicated, apparently some blue and green fluors stay in nonpolar regardless of pH and solvent so we might lose some with this first wash.

Very concerned that acetone might not hold too much magic, probably because other things like fats prevent it to. It takes too much solvent all around.

Following Kash tek also got final nonpolar freebase rather cloudy. Overall phase separation in steps was problematic. End product was gooey light brown with white-blue-greenish fluor, distinctive indole smell if there is such a thing. Yield was 0.27%, from 5 g fresh HBWR (like picked in the day). Did not allow it to fully dry, resuspended in 75% ethanol with fumaric (actually fumaric water first, good shake then etoh). Took a while to dissolve. Result is white-blue fluor liquid. Beautiful. Spent seed mush in acetone continues to give out fluor. continues

A previous extraction did the acetone freeze and feedback that acetone into more extraction repeatedly seems to have pulled more fluor and formed little emulsion in separation steps. End product was similar to before. Similar yield, less solvent spent, less of a hassle.

Some blue and green fluor stays in the aqueous and nonpolar phases at every step, it's just masked by each other and other junk. Wouldn't mind overshooting the pH to quickly pull it to nonpolar if it increases yield. Wasn't there a discussion with getting white instead of jungle dmt doing the pH up with the nonpolar mixed? did you do tlc on the solvent fractions in the other steps? There is a paper on the hbwr seed extraction content and their tlc also showed two spots, they ran it with lsd as standard.
 
Ruffles
#118 Posted : 5/17/2023 2:38:22 AM
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Here's the paper: Barone, Elisabeth, "Analyzing the Lysergic Acid Amide Content Extracted from the Seeds of Argyreia nervosa via the Use of LC-MS" (2021). Forensic Science Master's Projects. 5.

What you showed in your tlc fluor is that the top spot is most likely lsa, whatever the green one is, it is also an indole according to the paper.
 
Brennendes Wasser
#119 Posted : 5/17/2023 9:23:59 PM

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Quote:
What you showed in your tlc fluor is that the top spot is most likely lsa, whatever the green one is, it is also an indole according to the paper.


Thanks for the info! It seems it really runs much higher on a TLC than most other alkaloids, but the blue colour is then still a proof Surprised

Regarding your other idea about doing a Defat first: Seems also pretty smart as this seems to be also the go-to method for home chemists.

I had this paper dug up after I got no product during the extraction and here they also try a "Street Method". I put it into the collection and then overwrote this file from another one, now I cannot find the original one online again, as I'm in a hurry Sad((

Maybe will search tomorrow, but interestingly the "Street method" and their compared method was not too much different.

I think it was not a scientific paper / communication but rather a lab project with 40+ pages that was simply uploaded on their institution webpage.


Both ways that by

1. Curshing seeds to fine dust
2. Defat with Naphtha (so first catching up the oils seems smart)
3. Extraction with Acetone BUT already add small amounts of tartaric acid here.

No idea how it continued, but maybe it's also smart to try that way.

In any way it was a mix of alkaloids and LSA was only 0,13 % of whole seed weight, but that seems about right. Guess that's why I had nothing left based on a 100x seed starter pack. But regarding having a mix of Alkaloids, guess it does not matter as there will be no easy way of separating them. Also same amount of Iso-LSA already inside the plants present with their analysis.
 
Ruffles
#120 Posted : 5/18/2023 2:08:10 AM
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the project document is still up online.

Can you elaborate further on...

Quote:
It was told to not overshoot on pH as at > 10 it would induce creation if Iso-LSA. But I read in a paper they found even more Iso-LSA than LSA already in the plant. Probably would not favor the creation of even more Iso-LSA, but both are Diastereomers (only 1 out of 2 chiral site is changed) and so one could be sterically favored. But as I see it it should be the regular LSA as the Amide is in Cis position to a Hydrogen (small residue). Maybe then this problem would only arise when you already start with a pure Lysergamide, like what you would have on a LSD Blotter?


You mean an extraction is getting iso from the seeds and not converting lsa to isolsa?
 
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