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Methods of extraction... Options
 
AlbertKLloyd
#1 Posted : 12/8/2012 1:39:46 AM

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A while ago I harvested phalaris grass and did a simple extraction and got some spectacular crystals. However I did not try them because I had no idea what they were. Furthermore I then moved and the extraction was thrown out.

It got me thinking though, what if what I obtained was ideal? So I chose to try the same method with MHRB to see how it worked and it did.

I have not seen this particular method anywhere, despite elements of it being in widespread use.

I believe it is a good method for grabbing many things, including things like bufotenine and 5meo.

The plant material is obtained and then boiled, I prefer microwaves but for the phalaris I used a stove and pot. Add some acid, vinegar works fine. Basically you make an acid tea from your plant material. You will want to filter coarse material from the tea but fine material is ok.

After you have a good tea type material you reduce it in volume, one can use a microwave or a stove, but be careful because this method essentially requires all of the moisture to be gone, you reduce the tea to a dry residue. However before it gets totally dry you add some calcium hydroxide, though even baking soda works, you want your residue from your acidic tea to be made basic, not exactly caustic though, this isn't to break things down or allow an NP phase transition.

So the tea is reduced and made basic, this works well in the microwave but the last little bit might bump and splatter so once it is nearly done you can either let it dry out on its own or you can use a double boiler method to finish, a good method is to put a round glass bowl on top of a pot with some boiling water in the pot, put the thick residue from the tea in the bowl and let the heat from the boiling water dry it out all the way.

So now you have a funky residue, it is dry and maybe smells strange. Don't crush or break it up into a powder, leave it as it is, however take some 70‰ isopropyl alcohol and cover the residue, at this stage I sometimes heat the alcohol, but not always. I let it sit for some time and the alcohol changes color. Next I remove the alcohol. Now I have broken up the residue in the past, what happens is that some sediment kind of material then becomes suspended in the alcohol, so the solution if you have to deal with this is to put the alcohol somewhere to let it settle, the sediment will settle to the bottom of your container and you can decant the alcohol.

I don't know if all the steps are important, but what I have been doing next is to take the alcohol solution and put it into the freezer overnight. It seems that more stuff settles this way, perhaps plant waxes? Don't know... But I decant the alcohol again, pouring it off of the sediment that has settled in the freezer.

Next I take the alcohol and evaporate it slowly. As it dries out crystals form...

In the case of MHRB you will get an oily residue and crystals, evidently some of the alkaloidal material does not crystallize so well and stays very oily.

The AB and STB approaches don't work too well for some alkaloids, like bufo... But a tincture alone grabs too much, fats and waxes etc. This method here is a lot like an AB, but you do not use NP, you must dry your acid phase to a residue, before using alcohol as a solvent, and my best results used the freezer as mentioned.


In a nutshell what you would need aside from glassware or kitchen stuff is some lime, aka ca hydroxide, some 70% rubbing alcohol, some vinegar and your plant material. A freezer and microwave and all that is very handy too.

I like this method because it works well, uses very easy to obtain materials and it grabs alkaloids that are unlikely to be obtained using the more conventional methods.

I am hesitant to call this a tek, and sure don't want to be known as an author of a tek, but it works well and I don't know of anyone else doing it.

I had also seen crystals of mescaline obtained in a very similar way, but without the addition of acids or bases, just make a tea or juice or blend the cactus finely, filter, reduce to residue, cover with alcohol, chill, decant, evaporate... However this method does seem to grab things like tyramine variants and other such things that do not normally make it into a tea because they tend to not be very soluble in acid solutions. The crystals are also of the natural acids found in the cacti, not HCL or sulfates... They are interesting to see.

Goodluck.
 

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Parshvik Chintan
#2 Posted : 12/8/2012 4:33:24 AM

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correct me if i am wrong, but i thought phalaris extractions were supposed to isolate DMT from potentially harmful tryptamines?

if this is a more full spectrum extract i can understand one wanting to do it with mimosa or other orally consumable plants.

is there something i am missing?
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AlbertKLloyd
#3 Posted : 12/8/2012 4:55:48 PM

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Parshvik Chintan wrote:
correct me if i am wrong, but i thought phalaris extractions were supposed to isolate DMT from potentially harmful tryptamines?

if this is a more full spectrum extract i can understand one wanting to do it with mimosa or other orally consumable plants.

is there something i am missing?

Investigation extractions are not the same as extractions for use. Phalaris arundinacea can have so many things, hordenine, gramine, various betacarbolines, dmt, nmt, 5meo variants of those, I suspect fresh material may have some bufotenine as well given the odor of the extract.

I was investigating a very interesting patch of phalaris, which can frequently have the 5meodmt as the main alkaloid, conventional methods of extraction fail to obtain this. That and I was trying to see if this methodology was effective, and it was.


 
AlbertKLloyd
#4 Posted : 12/8/2012 7:09:53 PM

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When I did the MHRB with this method I used 10 grams and got a yield that I could not weigh easily due to the oily nature of it. So I have not weighed it... However visually the yield does seem higher than average.
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AlbertKLloyd
#5 Posted : 12/8/2012 7:16:43 PM

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Unless you hold the dish and move it, you cannot see that the oil is laden with tiny crystals, likewise the specks are little crystals that have formed. It is hard to see here, but this is the best I can do right now.

I would wager that the yield of oily and crystally material is a bit over a gram...from 10 grams MHRB. I wonder how much of the oxide of nndmt is left behind with other extraction methods... (Edited to add that this does not suggest an alkaloid yield of a gram, just that the residue obtained this way, which does contain visible crystals, was in the neighborhood of a gram.)

This method does work well, that is the only reason I posted it.

Also you need very little ca hydroxide aka lime, very little. FYI something less than a teaspoon is plenty for most reduction residues.
 
AlbertKLloyd
#6 Posted : 1/27/2013 7:49:30 PM

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It is almost two months later, here is an update on the MHRB residue obtained using this method.

The material is still mostly an oil like residue, the crystals have stopped growing, you can see them poorly in the photograph, they are much lighter in color than the oil, which has grown darker with time. The crystals are the specks that are lighter in color and in some parts of the picture are reflecting sunlight.

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AlbertKLloyd
#7 Posted : 2/16/2013 9:02:11 PM

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Quote:
Furthermore I then moved and the extraction was thrown out.


Not the case actually.

I found it.

this picture is terrible, but I will explain it, the sparkles are crystals from the Phalaris. When heated it smells a lot like bufo, effects are noticeable with VERY small amounts and it seems that the crystals may be 5meo...

I don't have a camera that will focus on this properly right now, the scale is that the crystals are about 1mm across and the bottom of the dish where the crystalline residue is is 5cm across.
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AlbertKLloyd
#8 Posted : 2/16/2013 9:15:46 PM

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Quote:
The other day I went and harvested fresh tips (1st 2-3 leaves from the top) of Phalaris arundinacea, simmered them with a dash of citric acid, reduced the brew, filtered, evaporated to a residue, did an alcohol extraction of the residue, reduced that, filtered that and reduced again to a residue, then I added baking soda (decent amount, to get to pH 10 or so) and water, then I reduced that to a residue and did another alcohol extraction of that residue.

I wanted to make sure I got a rich alkaloid spectrum and the plants I chose came from a population with a lot of genetic diversity. The resulting substance is reddish in mass, but thin sections of it are bright fluorescent yellow. More interesting, it smells like a yopo extraction, it smells like bufotenine!


I targeted a stand with a huge amount of visible biodiversity and selected fresh tips with reddish and purplish tones primarily. It was like harvesting tea, the total volume of the material was about 3 quarts worth of top leaves when compressed hard into a plastic bag. To gather this took about 2 hours and was somewhat tedious, but the whole plant is not worth messing with, only the upper leaves contain appreciable alkaloid content according to several studies.

The mild euphoria of a very small dose of this material inhaled when vaporized lasts over ten minutes.

I will also note that the yellow color gave way to a much darker reddish color over a few months, indicating some oxidation may be taking place.
 
jamie
#9 Posted : 2/16/2013 10:26:14 PM

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yeah that looks about right..same as the stuff I have extracted and smoked. What time of year was it harvested? I have had alkaloid profiles that seem to change based on my bioassays..there was usually tryptamine like effects present though..once it was very very potent but lacked much visuals. Definatly worth investigating more. I just went for a long walk through the forest here to some of my phalaris spots and found it all starting to grow back now as it's warming up..

I was using a similar tek..brewing the grass, filtering it and reducing down to a wet thick resin and basing it with lime..and then pulling with hot limo and salting. I also did a simple iso extraction on the based goo and decanted it numersou times and then evaporated and still had effects form it when smoked. I did another one pulled with hot olive oil but I forgot about it in the back of the fridge last summer and am too afraid to touch that stuff now..I will start again

I only bioassayed maybe 4-5 different extractions over about 2 years time from grass around my area, but I never flet anything subjectivly that I could link to bufotenine. If it is in there I would think it is negligable..I never got any of the kind of nausea I associate with bufotenine..I never had the guts to really smoke a good chunk of the extract though either.
 
jamie
#10 Posted : 2/16/2013 10:50:44 PM

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Here is another similar tek I did with chaliponga..

https://www.dmt-nexus.me...spx?g=posts&t=38641
 
AlbertKLloyd
#11 Posted : 2/16/2013 11:19:25 PM

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I didn't feel any effects like Bufo at the low dose, bufo has been reported in fresh grasses of some phalaris species but not in the dried, and I did process fresh grass, the smell is like yopo, but the effects are not so far.

I harvested in late summer/early autumn

Thank you for the link and information. I used this same method for the delopsperma spp and got needle like crystals but they only had mild stimulant activity.

I harvested a rather significant quantity of seed from the same stand of Phalaris, and it showed considerable variation in the plants, indicating some genetic diversity in the area, which is why I targeted that specific stand.

I am certain that my extracts produced this way contain alkaloids but do not contain only alkaloids, for more pure material standard methods of recrystallizing should be employed, the material produced this way (not the crystals but the residue) clearly has some carbon in it and does not vaporize cleanly.
 
AlbertKLloyd
#12 Posted : 2/16/2013 11:41:47 PM

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LOL, I made an error in judgement, the visible crystals in the phalaris extract are salts, this is what the flavor tells me, it tastes like table salt!

nothing special, the oily goo like material is however clearly what is containing the alkaloids causing effects in this case.
 
Jagube
#13 Posted : 6/18/2019 4:03:54 PM

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A couple of questions about AlbertKLloyd's tek from the OP:

1. Is there a difference (efficiency, selectivity) between using 70% IPA and 99% IPA?
2. After pulling with IPA, can one use FASI precipitation? I'd rather avoid evaporating the IPA. If one can just add fumaric acid crystals to the IPA pull, dissolve them and obtain fumarates, that would be a tek that doesn't use NP solvents or evaporation, and the IPA could be reused indefinitely, right?

If the answer to #2 is no, one could always pull with limonene like jamie and do FASI on that.
 
benzyme
#14 Posted : 7/4/2019 11:38:34 PM

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Jagube wrote:
A couple of questions about AlbertKLloyd's tek from the OP:

1. Is there a difference (efficiency, selectivity) between using 70% IPA and 99% IPA?
2. After pulling with IPA, can one use FASI precipitation? I'd rather avoid evaporating the IPA. If one can just add fumaric acid crystals to the IPA pull, dissolve them and obtain fumarates, that would be a tek that doesn't use NP solvents or evaporation, and the IPA could be reused indefinitely, right?

If the answer to #2 is no, one could always pull with limonene like jamie and do FASI on that.


1. Yes. 70% IPA contains more water, making it more polar, and thus it will pull more molecules that have polar side groups..hydroxy, ester, aldehyde, etc.

2. Yes, hypothetically. Fumaric acid may have difficult solubility in IPA; heating helps. I use a vortexer, then an ultrasonic bath to get it to dissolve. The latter is immensely useful.

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