Extraction of Mimosa Hostilis by Yoda's Method

java · Consumer

Methrix
(Stranger)
05-26-00 04:50
No 9550
      Yoda's instructions wrong ?

I tried to extract the alkaloids from Mimosa Hostilis. (by Yoda's method)
I ended up with what should be the solvent (DCM) with alkaloids, but was a dark brown almost black thick muddy substanse, I don't know where it went wrong.
I started putting the crushed rootbark in an acid solution of pH 1, it was there for 4 days, the filtred bark was put in a new acid solution for about 10 days. I combined the two filtred solutions.
I've read that it was best to do a defat process as it would make crystals rather that an oily gel substans.
So i added the acid solution in my sep funnel, poured about 5-10 mL DCM within. Shaked and waited a few minutes.
Whats wrong ? I thought.
The DCM at the buttom was not clear but was thick an fatty. So my guess was that it probably was fat and i discarded it, and added more DCM, it was the same result. My conclusion : That how we do a defat.
So i made it alkaline with NaOH lye, my indicator strips, was miscoloured as the solution had become almost black, and i wished that i had bought a pH meter too. Well i stopped when i was almost sure with a pH 11.
I'm not sure but i think the solution was room temerature when i added it to my sep funnel.
I continued adding an equal volume of DCM in the funnel, shaked, shaked, and shaked. I took a nap, and went back couple of hours later, what i saw was the alkaline solution on top, and the layer below was the muddy substanse which i discarded at the tragic ending.
I really hope someone could tell where i went wrong, cause i have about 200mL acid with tryptamines (hopefully) left.
-Methrix

jsorex
(Newbee)
05-26-00 06:10
No 9570
      Re: Yoda's instructions wrong ? Bookmark

If you shake DCM hard, you have to wait REALLY long to get clear seperate layers. DCM goes to the bottom. It is the bottom layer, unlike naptha which floats on water. What went wrong? Why are you not pleased. Did you get active oil. Or are you not happy, because you didn't get crystals?
Dcm is effective but may pull other crap along. So take the black oil, and put it back in to acid water and do the entire extractio again with another solvent, naptha. Then wash with water.
-jsorex

gnrm23
(Stranger)
05-26-00 06:44
No 9580
      Re: Yoda's instructions wrong ? Bookmark

after agitating the basified solution with dcm, the alkaloids should migrate into the organic layer (dcm, bottom layer)... the goodies were in the last dcm, apparently discarded (?)...
don't you folks ever sleep?

Lysergic25
(Stranger)
05-26-00 08:13
No 9624
      Re: Yoda's instructions wrong ? Bookmark

SWIM always did many a naphtha run of the acidified solution to insure that all the plant fats and oils had been cleared away. Then, when the solution was basified, there was hardly any gunk in the non-polar layer.

Maighstir
(Stranger)
05-26-00 23:35
No 9905
      Re: Yoda's instructions wrong ? Bookmark

I agree with the DCM comment. Use naphta, it works better with DMT extractions (at least for me; I only use DCM in final extractions, never in the first cause there's just too much shit in the mixture). Also, Yoda's method is perfectly OK.....for some plantmaterials. You must be carefull with extreme pH values cause some plants can give you a lot of trouble. If the pH is too low or high you could end up with thick gummylike mixtures because of the proteins present which precipitate. Some other plants will not do this, it's a trial & error process. The same problem could arise with other plantstuff (resins).
Vae victis meretrix est et mors venit.

catharsis
(Hive Bee)
05-28-00 14:15
No 10443
      Re: Yoda's instructions wrong ? Bookmark

would yodas method be worth while with a shit load of phalaris grass? i know it works with illioneseus..
-------
purge the info.

jsorex
(Hive Bee)
05-28-00 23:18
No 10607
      Re: Yoda's instructions wrong ? Bookmark

Yes, if using acetic acid, notice that DMT acetate is soluble in chlorinated solvents. You'd want to use naptha for the defat.
-jsorex

Methrix
(Stranger)
05-29-00 04:58
No 10683
      Re: Yoda's instructions wrong ? Bookmark

Ok, so i'll go get some naphta fluid.
Hopefully it's the Zippo lighter fluid you mean, cause i've found that naphta is a pretty common chemical in lots of solvents at the hardwarestore.
I appreciate your help, and i wont use DCM for DMT extractions in the future, Thanks !!
-Methrix

catharsis
(Hive Bee)
05-30-00 17:22
No 11484
      Re: Yoda's instructions wrong ? Bookmark

they sell big ass cans of naptha at hardware stores where i live. but if you cant find it there..try Rosonel or whatever lighter fluid..thats naptha. Yellow bottle. get it at a gas station. or grocery store in tobacco section..
-------
purge the info.

jsorex
(Hive Bee)
05-31-00 00:15
No 11626
      Re: Yoda's instructions wrong ? Bookmark

Aren't Zippo lighter fuels usually pet ether? That should do.
-jsorex

Dick_Fitzbetter
(Stranger)
05-31-00 14:24
No 11913
      Re: Yoda's instructions wrong ? Bookmark

About a year ago I did that Yoda extraction on an oz. of Mimosa Hostilis rootbark from BPC. It worked out pretty good, yeilding an orange, oily, wax-like product that was highly fucking active. I didn't do the defatting step at all. Just a straight a/b extraction using DCM. The only surprise (to me) was that it took between 24 to 48 hours for the DCM to fully settle out of the basified solution. I'm thinking maybe you didn't didn't wait long enough, because for me, at first that DCM layer was so muddy-looking you really couldn't see any dividing line between it and the aqueous, and I thought I had this terrible cluster-fuck of an emulsion that would never separate. But after 24 hours or so the DCM layer began to resolve and turn clear. At 48 hours it was completely clear, with only a slight yellow tint.
I'll never forget that plastic, burnt-rubbery smell. DMT is a serious mind bender. At the height of one trip I came pretty close to losing all concept of humanity, which scared the shit out of me. Thank god the trip is short. I might try it again sometime, but not real soon.
ô¿ô

IndoleAmine · Dreamreader Deluxe

Cover 100g finely powdered root bark with just enough dH2O acidified to pH 3-2 with HCl. Simmer (gently cook) for 2 hours, decant acidic water through a vacuum buchner filled with lots of celite to collect a clear, reddish-black liquid. Repeat this boiling/filtering process 2x with fresh acidic H2O.
Combine the acidic extracts, filter them again until it doesn't get cleaner anymore, and boil down to 1/3 of original volume using a pH meter to continuously monitor the pH. If it becomes lower than 2, add some sodium bicarbonate or similar to maintain pH between 5 and 2 (must stay acidic, but not below pH 2!). Alternately, use the combined extracts as is, but then you'll need more solvent for the next steps.
Defat the whole garbage by carefully extracting with chloroform/DCM 3x (don't shake too vigorous here to avoid emulsions) followed by 1 wash with a little ether. Collect the CHCl3 washes for recycling the solvent.
Prepare a 10% NaOH solution, and add it slowly to the whole gunk with good stirring, until it first turns from red to greyish/pink and then suddenly to a deep, ugly BLACK. This is where you want the pH to go: above 12.5. Now extract the whole thing with Et2O 3x, combine the ether extracts, wash with sodium carbonate solution, then with water, then with brine. If you want, you can re-extract with pH2 water, defat once with chloroform, once with ether, basify again and extract again 3x with ether and evaporate that to get ultra-clean product.
Or if you're not in a hurry, you can place the ethereal extracts in a small RBF after washing, distill away most of the ether (caution!!) and transfer the remaining dirty N,N-DMT residue to a small evaporating dish using a little more ether. After several days, little hexagonal crystal columns will appear, and BTW: you will realize a distinct "burt rubber"-smell in your evaporating dish if your dream was successful...

(yield is 0.11g from 25g root bark BTW)

Oh, and just to clarify about the uncommon choice of solvents: solvents other than diethyl ether and chloroform CAN theoretically be used, but in several dreams naptha, hexane AND pet.ether formed nasty emulsions and seemed not to be very selective for the defatting stage. Toluene was tried for defatting and found to be good, but the disadvantage with such high-boiling solvents is their long evaporation time compared to Et2O, so the dreamer who told me about this dream decided to use Et2O for the final extraction. Chloroform was choosen because virtually no emulsions formed when defatting with it. DCM should work just as well.

And to finally answer your pH question: normally, a pH around 10 is sufficient for basifying DMT salts. BUT this is only the case when the salts are present in a clean aequous solution. What you have after MHRB extraction is everything else but a pure salt solution. The high pH value of >12.5 assures that much of the crap becomes soluble in the aequous phase again. When you basify to pH10, you'll have to do a lot of washing, and N,N-DMT is stable even in pH12.5 solutions, so there is no loss in yield when aiming for a pH >10, I would rather say that with pH10 you'll get less DMT, because some will be lost in the successive water/bicarb/brine washes..

So: Use toluene for defatting, but a low-boiling nonpolar for final extraction, also make sure to remove toluene traces with your low-boiling np BEFORE basifying. And hit pH 12, make it turn black. Don't stop adding lye before there is no more color change anymore. Then success is almost guaranteed.

(copied from our friend site WD)

IndoleAmine · Dreamreader Deluxe

I know someone who knows someone who has dreamt about extracting 100g MHRB recently, and I was told that he got 0.9g (!) only from the first extraction of the pulverized root bark. He used 0.01 N HCl (8.3ml 37% HCl diluted to 1000ml), and ~600ml were needed to cover the dry root bark at the beginning. For basifying, he used 12.5g NaOH dissolved in enough H2O to make for a total volume of 250ml (this is a 1.25N NaOH solution) to avoid having local peaks with pH>13 build up; these peak concentration could otherwise destroy some alkaloids (so: don't use solid NaOH here!!). The root bark was stirred magnetically at 90°C for 3 hours and then the reddish-black solution was filtered 3x through the same bed of celite, until it came thru crystal clear. Now the whole thing was shaken vigorously with 100ml CHCl3 - emulsion. Again filtered through same celite pad - cleared up, 2 layers (nonpolar slightly yellow). Repeated with fresh 80ml CHCl3, resulting in not as much emulsion. Filtered through celite, separated. Washed with ~30ml Et2O, then basified by adding the premade 1N NaOH soln. with swirling gently until it was black like soy sauce (good comparison!), then added a bit more lye, and covered with 300ml Et2O. Shake carefully while venting often (!), let sit for about 30 minutes. Most of the emulsion clears and the ethereal layer appears clear. separated, washed the Et2O with dilute NaOH, then saturated NaHCO3 soln., then brine, then water (the washings subsequently become cleaner with each wash), then dried with Na2SO4 and the ether evaporated on a rotovap. Returned the ether to the black pH12.5 soy sauce and extracted again, washed and removed solvent using the same evaporation flask still filled with that yellow oil remianing from the first extract. Repeated extract/wash/evap process until the black solution had been extracted 5x. Transferred the yellow oil into a small porcelain evaporating dish using a little more ether to rinse the flask, and set aside. After 2 hours, little crystals began to form, and SWIA being impatient (and wanting to leave lab after 10 hours of working with nasty solvents) scraped the oily mass together with razors, smeared it on a glass plate making a very thin film, scraped it together again, smeared it onto the plate again and suddenly, it solidified into a yellow-orangish amorph crystalline mass, total weight after drying: 912mg (!!)

(also copied from WD)

IndoleAmine · Dreamreader Deluxe

And another important thing to consider when choosing the solvent(s) for mimosa hostilis alkaloid extractions is that haloalkanes (like DCM and chloroform) seem to cause some of the N,N-DMT to cyclize into a tetrahydro-beta-carboline under basic conditions, and this compound is known to act as a MAO inhibitor just like harmaline does. In other words: instant ayahuasca experience instead of a clean DMT high. (!)

see also this interesting thread over at the bluelight forum:
http://www.bluelight.nu/vb/showthread.php?s=&threadid=177688&r=10
(thx again Java!)

have a nice weekend

i_a

IndoleAmine · Dreamreader Deluxe

Why? The problem is that haloalkanes can form aldehydes (acetaldehyde/formaldehyde) upon coming in contact with a strong base.

If you basify the whole acidic extract, you create severely basic conditions, and if you use a haloalkane like DCM or CHCl3 for extracting this basic aequous phase, you can be dang sure that your solvent comes into contact with a strong base. And eventually some formaldehyde is formed.

The only remedy I can think of would be to use no DCM or similar when extracting the basic aequous phase - washing the nonpolar extracts only reduces the contact time, the problem of a side reaction occuring isn't solved this way.

Luckily naphta, pet.ether and the like are cheap and contain no haloalkanes, hm? Wink

IndoleAmine · Dreamreader Deluxe

anyway..

here are some interesting links about tryptamines in general and DMT in particular:

http://userpages.umbc.edu/~jfreed1/lsdrecords/trypfaq.htm
(good reference about active dosages of many exotic tryptamines)

http://jeremybigwood.net/JBsPUBS/DMT/pages/DMT1.htm
(six-page article about DMT, by J. Ott)

http://www.maps.org/news-letters/v04n2/04230cal.html
"Tryptamines, Beta-carbolines and You", J.C. Callaway
MAPS - Volume 4 Number 2

http://www.erowid.org/chemicals/dmt/extraction_guide1/dmt_extraction_guide1.shtml
(QT's DMT extraction manual)

http://elfspice.tripod.com/acacia/acacia_extraction.html
(Elfspice's complete N,N-DMT extraction guide, with pics)

http://www.erowid.org/chemicals/dmt/dmt_chemistry1.shtml
("Yoda's DMT extraction action")

http://ethnobotany.yage.net/extraction.html
(another extraction)

i_a