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The Quest for the Best Mescaline Extraction TEK Options
 
AlbertKLloyd
#21 Posted : 9/6/2012 2:44:17 PM

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I am surprised to not see STB and microwave assisted extractions on the testing list.

I suspect microwave extraction will be the fastest and easiest method. I've used versions of it for a couple years now with lots of success, including with MHRB extractions and it is very quick and yields very well.

If you combined a drytek method (damptek more likely) with a microwave you could probably be at the salting stage very quickly. You would take your dry cactus material, hydrate it with some caustic solution containing lye or lime, cover it with an NP like xylene, mircowave for a few minutes, decant off the NP, filter it and begin salting out the alkaloid. You could have a solution of alkaloid salts in about an hour easily and have an extraction efficiency like only microwave extractions have (90%+ in minutes)

still i like the comparison here.
Good work Mew!

 

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endlessness
#22 Posted : 9/6/2012 2:57:52 PM

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I dont think it's a safe recommendation to microwave flammable solvents. Even if yours worked fine, you never know with electric equipment and possible sparks, who knows what kind of microwaves other people have. I dont want people to blow themselves up by following something they read on the nexus.

Microwaving an acidic aqueous solution of your plant matter, though, seems more reasonable.
 
AlbertKLloyd
#23 Posted : 9/6/2012 3:10:31 PM

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You have a good point, there is a potential risk, but perhaps less than it might seem.

NP solvents are typically not affected by microwaves, microwaves pass right through them (they are microwave transparent) and don't heat them up, this is why electromechanical separation of alkaloids and plant material occurs. Since NP solvents don't heat up and evaporate in the microwave a container with a lid can be used, assuming it is microwave transparent.

Microwave extractions using NP solvents are commercially and scientifically employed now on a widespread basis and are considered the most efficient and quickest methods of extraction.

There is no point in microwaving the acidified solution other than it might be faster than the stove. Since the acid solution is not microwave transparent it heats up and this defeats the point of the microwave method.
These detail the methods and principals of microwave extractions.
h++p://scialert.net/fulltext/?doi=rjmp.2011.21.31&org=10
h++p://www.sineo.cn/pic/article/42.pdf
h++p://www.cem.de/documents/pdf/RE/RE014.PDF

I could not just let a thread with this title go by without a mention of what I think is the best extraction methodology so far.



 
mew
#24 Posted : 9/6/2012 9:16:16 PM

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thanks for the suggestions ill do method 2 with microwave pulls in the future since dlimo isnt that flammable



on another note the culprit too much acid salt was dissolved in ph 6 hcl water and filtered to yield about 20% less very clean light tan alkaloids, the cleanest salt mew has seen prior or post clean up
 
ntwhtyouknw
#25 Posted : 9/6/2012 9:20:46 PM

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I just don't see how putting xylene in a microwave is at all feasible. I tried to reduce a vinegar salting in the microwave from a limo pull in a mimosa extraction. I guess a tiny bit of limo carried over because I heard a loud POP, and I ended up cleaning jimjam out of the microwave. I'd hate to imagine if I were to put solvent intentionally into the microwave.
Toadfreak!

Travel like a king
Listen to the inner voice
A higher wisdom is at work for you
Conquering the stumbling blocks come easier
When the conqueror is in tune with the infinite
Every ending is a new beginning
Life is an endless unfoldment
Change your mind, and you change your relation to time
Free your mind and the rest will follow
 
mew
#26 Posted : 9/6/2012 9:31:48 PM

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it was your vinegar that popped, you cant let it go on for too long or it boils insanely
from what albert says, the dlimo will remain relatively unaffected, minus conduction heat via hot salt solution


i reduced vinegar saltings once and had to turn it off for a few seconds every few seconds to not let the evaporation turn into a total mess
 
ntwhtyouknw
#27 Posted : 9/6/2012 10:00:59 PM

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Ah, I stand corrected. Still I can't say ill be putting any solvents in the microwave.
Toadfreak!

Travel like a king
Listen to the inner voice
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Conquering the stumbling blocks come easier
When the conqueror is in tune with the infinite
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Life is an endless unfoldment
Change your mind, and you change your relation to time
Free your mind and the rest will follow
 
mew
#28 Posted : 9/6/2012 10:12:37 PM

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i have a designated microwave in a bomb shelter remotely controllable, i might give it a go ....
lol
 
ntwhtyouknw
#29 Posted : 9/6/2012 10:51:38 PM

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Well I have to admit I'm more than I little curious about it now.
Toadfreak!

Travel like a king
Listen to the inner voice
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Conquering the stumbling blocks come easier
When the conqueror is in tune with the infinite
Every ending is a new beginning
Life is an endless unfoldment
Change your mind, and you change your relation to time
Free your mind and the rest will follow
 
DiMiTriX
#30 Posted : 9/6/2012 11:07:04 PM

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great experiment fella!! Very happy
Tz'is aná
 
Kash
#31 Posted : 9/7/2012 12:28:04 AM

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mew wrote:
so what do i want, ph 2-3 (1%) or 5-6 (?%)

could you explain more about the reason for 4-5% acetic acid so i can extrapolate that info and apply it to fumaric acid aswell, this is the type of info im looking for Smile

Final pH 2-5 is fine using 1 % hcl. If pH is higher Swim worries not all alks are converted to salt form and that some may still be present in np.

To form mesc acetate you need 1 mol of acetate ions to link with 1 mol of mesc, plus alittle more for the other alk impurities to link with. Reason for 5% acetic acid is because mescaline has molar mass of 211g/mol and acetic acid 60g/mol and assuming a yeild average of 1-3% of 100g powder at most then 3g X 1mol/211g X 1:1mol ratio X 60g/1mol = .85g acetic acid needed roughly. Since acetic acid has a density similar to water then 4-5% acetic acid would contain 4-5g acetic acid per 100ml soln which isnt too overkill from .85g. I suppose you could use more dilute 2-3% but SWIM would be paranoid alks are being left in the np lol.

Fumarate ions may tend to form two bonds with stuff so you use a 1:2 mol ratio Razz
--------------------------------------------------*Kash's LSA Extraction* * Kash's Mescaline Extraction*------------------------------------------------------
All things I say are complete and utter ramblings of nonsense. Do not consider taking anything iterated from the depths of my subconsciousness rationally and/or seriously.
 
dg
#32 Posted : 9/7/2012 1:03:24 AM
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try titration, less separations, cleaner product
multiple acidic washes is a waste of time imho
 
AlbertKLloyd
#33 Posted : 9/7/2012 2:29:46 AM

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ntwhtyouknw wrote:
I just don't see how putting xylene in a microwave is at all feasible.

You didn't read the papers I provided links for. One of them has a graph showing heptane (not totally unlike Xylene)and a heating curve over time in a microwave, the heptane did not heat, it is transparent to the microwaves, so are many oils, like various veggie oils.

If you have worked with oil in place of Xylene before and can manage it (it can be tricky) then you could use that in place of the xylene, or whatever (limo etc) I don't know how D-limo acts in the microwave, test it before you use it if you plan on it... (of course!) and microwaves can facilitate some strange chemical reactions, you can use them to drive reactions etc. I really don't know of anyone (other than me) who has been exploring MAE (microwave assisted extraction) with psychedelic alkaloid containing plants, please consider it untested and potentially risky. Don't try it unless you are able and willing to research it in decent detail, otherwise you might be putting yourself in harms way.

Anyway sorry I brought it up, but too late now eh?

 
mew
#34 Posted : 9/7/2012 7:06:07 AM

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thank you kash for the knowledge, im glad its here now


thank you albert for sharing your experience and info with MAE, ill try it with method 2, my only concern is that the aqueous phase wont be mixing with the organic, so i asssume less effective yields (cant stirr while its in a microwave, could always take it out for a second and mix it up)

dg could you elaborate please, im pleased to see you posting. you have a wealth of information that would be most appreciated if shared (myself at the very least), many thanks!
 
AlbertKLloyd
#35 Posted : 9/7/2012 2:31:03 PM

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I'll note that microwave extractions are typically reported to reduce extraction times to something like 2-8 minutes, in comparison to 6-8 hours of reflux, and is generally much more efficient than the reflux methods, something like over 90%+ efficiency.

In the case of MAE the ultrasonic waves excite traces of water in the cells and create intense pressure, rupturing the cell walls and pushing the contents out of the plant into solution, this is electromechanical separation, as opposed to a gradual separation due to principals of osmosis and solute strength. In one 10 minute MAE run you can get more alkaloid from a plant than you could with repeated boiling or soaking methods! It is kind of amazing.
 
endlessness
#36 Posted : 9/7/2012 2:44:19 PM

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Yeah but with what microwave were the experiments done? Kitchen microwave? Or specialized lab microwave?

Also can you really guarantee everybdy's microwave will NOT have any sparks?

Please, be careful people, IF you will try this, make sure to be standing far away, maybe have goggles on, have a fire extinguisher nearby and dont have all sorts of extraction equipment or anything else drug-related standing around in case something happens and the firemen have to come in.
 
AlbertKLloyd
#37 Posted : 9/7/2012 3:54:53 PM

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Do not try a microwave method if you have not researched it in depth.

The extractions that are state of the art use special microwaves, but the older ones used conventional ones, which work, but you can't control as many variables with those.

The most dangerous solvent to use in a microwave is alcohol, things like xylene do not heat up, so you can put them in a sealed container in the mircowave and they won't give off fumes that can ignite. However with alcohol this is not true, it does heat up and fume and a spark could cause an explosion. If you want to try MAE you need to know exactly how your solvent reacts to microwaves, trial and error is not going to be ideal, just dangerous.

However with things like Xylene, a microwave might actually be safer than conventional methods because a lot of common methods employ heating the xylene, this makes it give off a lot of flammable fumes and a human being can ignite them with static electricity, or a light switch etc. With the microwave since the xylene is not heated it fumes less, however if you did put an open container of it into a microwave and a spark did occur then a fire could result.

http://www.cem.de/documents/pdf/RE/RE081.pdf
Quote:
It must be strongly stressed that using a
domestic microwave oven for laboratory purposes should
not be considered. Application of microwave energy to
highly flammable organic solvents may cause serious
hazards. Furthermore, reproducibility may be poor with a
domestic device because of the lack of homogeneity of
the microwave field. It is therefore seriously recommended
that only equipment approved for MAE be used.


However from the same paper:
Quote:
Sparteine, a lupine alkaloid, was extracted
from lupine seeds (Lupinus mutabilis) with methanol:acetic
acid (99:1, v/v) in a domestic microwave oven (see
caution above!), and the treatment (one to five cycles of
30 s with a cooling step in between) gave 20% more
sparteine than was obtained with a shaken-flask extraction
using the same solvent mixture for 20 min (Ganzler
et al., 1990).


In table two 7 of 15 results employed domestic microwave ovens.
 
endlessness
#38 Posted : 9/7/2012 3:58:22 PM

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Thanks for the info Smile
 
Kash
#39 Posted : 9/8/2012 1:22:35 AM

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So how are the experiments coming along mew?
--------------------------------------------------*Kash's LSA Extraction* * Kash's Mescaline Extraction*------------------------------------------------------
All things I say are complete and utter ramblings of nonsense. Do not consider taking anything iterated from the depths of my subconsciousness rationally and/or seriously.
 
mew
#40 Posted : 9/11/2012 1:20:29 AM

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with regards the methods 3 and 5

when using a powder and making a tea the best way to separate the liquid from the pulp is decanting/pouring. let settle and get a bit more out, finally when all that can be retrieved is homogenous with the pulp, add more water and let settle again.

this is definitely not something that can be rushed, easily

mew tried straining through a towel (it still squirted out powdered cacti pulp through looser weaves)
mew tried using a t-shirt (it got gummed up with super slimy dark green snot, then ruptured from pressure)
a fine mesh can be used if a cup is filtered at a time, the pulp can be set aside, for larger extractions the above decanting method is superior



the remainder of the pulp after a few water pulls will be bassified and pulled with nps to make sure there is no waste. from past extractions mew theorizes there will be a loss of nps due to the viscosity of the substrate, hence cheap xylene will be used in copious amounts

while the mescaline water will be filtered/decanted then reduced to make 1. water based resin (method 5) and 2. used in a typical a/b (method 3)
 
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