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Successful Virola extraction? Options
 
mycosis
#1 Posted : 6/26/2019 12:15:43 AM
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I recently sourced some seemingly good quality inner root bark of this tree and promptly began running some extractions on it in 200g batches. My first attempt was a variation on the BLAB tek. I substituted calcium hydroxide for sodium hydroxide. While I ended up with a lot of crystalized material in the end, none of it appeared to be the alkaloid desired. My second attempt left me with a small amount of dark tar that wasn't enough to test. That was a heatless, but extended A/B extraction using citric acid and basing with sodium carbonate. DCM was used for the pulls. Now my last and final attempt is an STB style. No heat was applied during this one either...rather I left it sit in my 100 F garage for three days. I elected to use sodium carbonate again...brought to a PH somewhere between 10 and 11. On the third day I added 25 ML of DCM. I then vacuum filtered this three times while running 25 ML pulls of DCM through it each time. In a separatory funnel, I did the standard shake and let settle procedure. Each time I extracted solvent for evaporation I added another 25 ML. I did four pulls of this and let it evaporate. I was left with a thin layer of dark red waxy material like you see below. Erlich test results, although impure, seem to be encouraging...as it turns out my filters are garbage; I also think applying heat would've cut back on some of the emulsions which found there way in due to my haste. I wish to share this with the community to receive feedback. I really do think applying heat next time will return a better yield and product. My new filters are on the way along with a soxhlet extractor which I know will give me better results. That being said, out of 200g of raw shredded bark, I was left with 220mg of final product. My impression is 5-meo-dmt extraction is not as tricky as it seems and that most of it amounts to the quality of the starting material. I welcome feedback and apologize in advance for not having more photos...I was about to give up on this bark.

Love and light,

mycosis
mycosis attached the following image(s):
erlich_1.jpg (2,427kb) downloaded 134 time(s).
erlich_2.jpg (3,127kb) downloaded 134 time(s).
erlich_3.jpg (3,126kb) downloaded 137 time(s).
 

Live plants. Sustainable, ethically sourced, native American owned.
 
endlessness
#2 Posted : 6/26/2019 12:46:25 PM

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mycosis wrote:
crystalized material in the end, none of it appeared to be the alkaloid desired.


Based on what it doesnt appear as the alkaloid desired?

mycosis wrote:

I added 25 ML of DCM.


DCM definitely works to dissolve the wanted alkaloids but it can potentially react with tryptamines, so I'd be careful with using it, if so, make sure you evap/salt as fast as possible, not leaving it in contact for too long.

mycosis wrote:

Erlich test results, although impure, seem to be encouraging...


Its hard to see from the pictures, can you please describe what color it changed to ?

mycosis wrote:

out of 200g of raw shredded bark, I was left with 220mg of final product. My impression is 5-meo-dmt extraction is not as tricky as it seems and that most of it amounts to the quality of the starting material.


I think that's exactly it, it's less about 5-MeO-DMT being fussy, but more about it being difficult to find good raw material to start with. You said Virola but never specified which specific species of Virola? Also, the indigenous people use the bark resin, not the bark itself, so it might be that the bark you bought had very little of the resin where most alkaloids are contained..

Are you considering bioassaying it anytime soon?
 
mycosis
#3 Posted : 6/26/2019 1:03:01 PM
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The first extraction's test was based on a bioassay (sublingual). I could've been wrong there as I didn't have the TLC kit yet.

Yea I've noticed DCM pulls a lot more than just the alkoloids...I think I will likely use acetone and then heptane to crystalize in the future (stick w/DCM for defats and such).

Immediately upon dropping one drop of the Erlich on the TLC strip, the outer edges turned from a light blue to dark blue/purple. It seems to be consistent w/a hit on 5-meo-dmt freebase. What concerned me was the whole middle of the affected area is just yellow. I've never performed this test so I don't know if that is normal. The outer edge that reacted looks good to me though.

Species of bark was Virola theidora specifically. I believe this is the inner bark before the resin is cooked out...it smells potent. Straight indole to the face when you open it up. (As it turns out so does this waxy substance I've created) The DCM was evaporated off completely within 2 hours. I erroneously attempted to freeze precip the first pull of it. Once I realized my error I scraped what did crystalize out of the beaker and stuck it in with the rest of the solvent from the other pulls. This was then evapped over a large pyrex dish w/fast running air over it from two sides (in my 100 F garage)

I did end up bioassaying this batch. 50mg sublingual. I don't think this stuff is active at that low of a dose but I was hesitant to go higher or smoke it until I got some feedback. I did notice a warm rush come on 10 minutes in that lasted approximately 10 min. I think I felt a slight afterglow that is reminiscent of the 5-meo experience as well. It tasted very bitter but did not burn. I was able to roll it up into a ball and place it in my mouth where it dissolved slowly.

Apologies...I didn't see the quote button until after the post.
 
endlessness
#4 Posted : 6/26/2019 2:49:22 PM

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Was it the bottom spot on the tlc plate that turned purpleish? What about the top spot?

If you can take a pic of the plate under UV light that'd help us seeing a bit more too.

Do you have any dmt-containng plant or dmt extract to test next to it?

Do you have any other reagents?
 
mycosis
#5 Posted : 6/26/2019 3:15:45 PM
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endlessness wrote:
Was it the bottom spot on the tlc plate that turned purpleish? What about the top spot?

If you can take a pic of the plate under UV light that'd help us seeing a bit more too.

Do you have any dmt-containng plant or dmt extract to test next to it?

Do you have any other reagents?



The three spots closest to the substance are the best samples...they are also closest to the bottom of the strip where the x's are located. I'm attaching a UV photo where they are on the left.

I have some changa and toad venom I could possibly test on...can I just toss a small amount of either into a test vial and give it a good shake like I did w/this?

I have the Marquis and Mecke reagents as well. I chose Erlich because it could differentiate between 5-meo and DMT easier so I figured it would be most sensitive.

Thanks!
mycosis attached the following image(s):
uv.jpg (3,277kb) downloaded 96 time(s).
 
endlessness
#6 Posted : 6/26/2019 10:06:33 PM

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Sounds like a great idea to test on one column the toad venom, on another changa, and on another your virola extract.. you can do this with 3 plates, one you later use ehrlich on all spots, one you use marquis, one you use mecke. Even if those other 2 are not the best to distinguish 5-meo from n,n, they could eliminate some other potential unknown substance that could be misleading the results... Its always good to test as many ways as possible.


And yeah, its as simple as toss a little in a vial with a solvent and test it. Smile

Thanks for sharing the results of your experiments with us!
 
mycosis
#7 Posted : 6/27/2019 12:02:06 AM
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I will post those results this weekend sometime. I must confess I am between jobs/roles currently for employment so regrettably I must focus my willpower on these types of endeavors. I promise to follow up...hopefully further testing will lend enough confidence for a more venturous bioassay. I made a commitment to my little toadies to find a viable plant based material for this magical substance as well as do everything in my power to ensure their survival, and I intend to uphold that commitment. I am eternally grateful to you, 69ron, and CaptainFuture for your contributions.
 
endlessness
#8 Posted : 6/27/2019 9:41:50 AM

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Hey friend, good luck on your job search! I know this struggle very well, it totally makes sense you dedicate your time to that. These experiments you are doing can always be done later on, no hurry!

Be well!
 
mycosis
#9 Posted : 6/28/2019 1:15:53 AM
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Quick update...I ran another test on all three with the erlich agent. I got two very positive results for dmt on the changa and 5 meo on the venom. (virola top, changa middle, toad venom bottom). Nothing came back on the bark extract this time. I did not wear gloves the first time... this is the only thing I can think of that might've interfered. I also did not touch anything recently but this bark and what i think is digitaris cilaris. I'm not giving up yet... just waiting on some specialized equipment for this last batch. I'm considering doing a STB rub with sodium carb and letting it dry, then running it through a soxhlet with acetone, and then pulling with heptane for crystalization. Either that or do the carb step after acetone. What do you think?

At least now I know what a strong hit looks like for erlich 😀
mycosis attached the following image(s):
tmp_20510-IMG_20190627_2003474592490615201550332.jpg (2,291kb) downloaded 68 time(s).
 
mycosis
#10 Posted : 6/28/2019 1:46:11 AM
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Duh, I handle my toadies almost daily to change their water, etc. That could be the possible mixed result from the first test. I'd still like to proceed with this last extraction and welcome any insight.

Thanks again!
 
mycosis
#11 Posted : 6/30/2019 11:20:57 PM
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Ran a soxhlet extraction on 100g w/ 750 ml acetone for 18 hours-ish. Based it with sodium carb and added 50 mL heated heptane to hopefully pull any alkaloids into that for freeze precip. Crystals did form overnight, but upon removal they quickly became a thin film of golden tar. I scraped this up and tested it with zero hits on erlich and a possible hit on both mecke and marquis for dmt only). I still have some raw material left, but I'm not really sure how to proceed. During this extraction I re-checked the label and it is actually Virola calophylla. From what I've read on the internet, this only has DMT. I can only surmise this product is bunk because in my experience, DMT extractions are ridiculously easy on barks and this shouldn't be any different. So I guess I bought a mislabeled product that was probably ancient. I can't seem to find a reputable source of seeds or seedlings for theiodora, but the tree would grow just fine in my climate (mimosa does very well). I will just focus my energy on the grasses going forward I think.

At least for posterity's sake, there's a documented test against known good changa and bufo a. venom. Big grin

blessings,

mycosis
 
 
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