Separating Resin into its components

[Phlux-]

This is part of an ongoing experiment, it will be updated as the experiment progresses.

The aim of this experiment is to yeild pure mescaline without using non-polar solvents - and preferably keeping chems used to naturals.

Cactus tea was prepared from 1.44kg of fresh torch, it smiled back as it should(stated in my cactus jelly tek - Phlux-'s Cactus Jelly Tek - Preparation - Welcome to the DMT-Nexus )

The tea was filtered then reduced

Acetone was then added to the tea

instantly the acetone caused precipitation, so it was stirred

the massive amounts that immediatley precipped were solid and stuck together enough to use a spoon to remove them from the tea

this was dried to yeild

this precipitate was tasted and didnt taste much like mescaline at all - its almost tasteless - perhaps a tad of mesc caught in there from the speed of precip

the precip was washed with water and filtered, a thick solid film formed on the plate and was scraped up to yeild very shiny xtals

water re-x'd on the right side of the plate - the rest of the uncleaned precip on the left

after precipitation the tea was watery, not syrupy at all, it was filtered with ease then evapped to yeild the bitterest tasting resin ever with a smell of caramelized sugar

the resin was washed with acetone - not much changed the acetone went yellow and something came off - not much tho - no change in color.
then it was washed with ipa and it turned into a beige powder when under the ipa, when it was dried off it instantly changed color back to dark, allthough when scraped, white appears on the surface.
The resin was then washed in mek

i beleave the mescaline is still in the resin and there is another alkaloid that is hygroscopic as hcl as the resin wets itself in a few hours.

i think the precipitate is cellulose, cellulose is water insoluble but suspends well in it and is able to pass thru certain filters.

the fact that the water purified filtered cellulose looks so much like mescaline explains this question i posted a few days ago on mescaline xtal structure ( Mesc types or stubborn contam - Preparation - Welcome to the DMT-Nexus )


found this here - http://www.patentstorm.us/patents/4042720/description.html
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Reference has been made to use of the cellulosic fiber as a stabilizer in various food products and formulations. In addition to being hydrophilic, it has the ability to absorb sugar syrup. Thus when the fiber is used in formulations having asubstantial amount of sugar syrup, during concentration by evaporation the fiber absorbs syrup simultaneously with concentration in a single cooking cycle (e.g., from 50 to 80 Brix in less than 1 hour). The resulting product is stabilized by the cactuscellulosic fiber, in that body is imparted which is retained for prolonged periods. When such impregnated fiber is used as a filling for bakery products, the physical form is retained during exposure to baking temperatures, and migration of moisturefrom the stabilized form to the adjacent cooked dough or batter is minimized, whereby moist eating properties are retained over extended periods of storage. Also when blended with a dough (e.g., 25% dry solids basis) it serves to reduce dough spreadduring baking and imparts moisture retention and chewey eating properties that likewise are retained over extended periods of storage.
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if this precip really is cellulose then it may serve as a good encapsulating material - as in the cellulose is melted down into transparent or colored sheets and mesc doses placed in pre-cut envelopes made from this.

im not quite certain how to separate the other alkaloids


I think this tek could lead to a total yeild as salting a nonpolar solvent containing freebase mescaline and pulling with hcl water seems to cause some degridation that can cause an apparent 50% loss, in comaprison to gassing with hydrogen chloride.

 

[Oncewas]

Very cool!

Go figure resin is encapsulating material and mescaline(and some negligable plant sugars).

Excellent work phlux! Looking forward to more advancements!

 

[Phlux-]

any ideas on how i can separate the mescaline contamination from my ?cellulose? i know cellulose is not soluble in a lot of things - perhaps the best bet is water and excellent filtering - vaccum filtering is now a nececcity it seems.

also any ideas on how to separate sugar from mescaline ?

 

[Phlux-]

The resin was evaporated down further - it drew so much moisture from the air in the past day.
The yeild was 12g resin, 12g cellulose nice even numbers (and 12 is my favorite number)

Here is the resin as it stands

 

[whiterasta]

This same algorithym is being explored in this THREAD @ the nook with a bio assay of the resin HERE. The poster thinks further reduction ay be possible with amylase enzymes perhaps or a strong acid to break any polysaccharides down to simple sugars. He also has posted pics of sectors of crystallization of distinct HCl fan crystals in the drying dish but they returned to a stiff tar when scraped up.
Even his natural salt resin showed signs of crystals in sectors. this implies given the right circumstances and some further work the resin may precipitate a crystalline product.
I do think his goal, from our conversations, is to retain all the effects of tea/syrup without using the standard base/salt teks which almost everyone agrees is not as full as the cruder extracts.
He has written an essay for membership here(soxy bastard) and IMO would benefit the conversation about this approach.
Yours,
WR

 

[antichode]

Its worth nothing Phlux, that if you dont blend your cactus when making tea the cellulose isnt there, at least not in any amount that you've shown above. The resin extracted from large chunks instead of blended has the same consitency as what you posted above.

SWIM has extracted resin both ways, and when he blended the cactus he ended up with a white fatty layer on top of the resin. When both the white layer and resin were evapped a canddy like resin formed that wasnt tacky at all. It attracted moisture a little, but the white layer seemed to keep the resin hard like candy, not tacky.

This didnt happen when he used chunks as in House's method. The resin made from chunks was far more potent by weight compared to the blended resin and white layer combined. The resin made from chunks remained rubbery and tacky.

Keep up the experimentation tho, its great to see your results

 

[Phlux-]

"Its worth nothing Phlux, that if you dont blend your cactus when making tea the cellulose isnt there, at least not in any amount that you've shown above. The resin extracted from large chunks instead of blended has the same consitency as what you posted above.
"

hehe dude this cant be true - reason being - THIS IS from thickly sliced peices of cactus, simmered softly, 2 pulls, 2 hours each, not ever pressed, just strained thru a collander.
I have made cactus tea now at least 100 times, iv tried blended, diced, chopped, mashed, everything, what you mentioned above about there being more with blended is true, but the results speak for themselves.

 

[antichode]

hehe dude this cant be true - reason being - THIS IS from thickly sliced peices of cactus

hah... ok then SWIM just put it down to the blended cactus as thats the only time he has ever had the white layer. But with 6 or 7 brews done so far he's a long way off swiys quota

keep working the mad experiments tho

 

[Crystalito]

Nice work there!

Well,how can we test if the first precipitation is cellulose? Anyway it seems that whatever it was is not active and was removed from the tar actually making it TWICE potent by weight.To reclaim any alkaloids that could have been trapped there you could try washing it with acidified water and vacuum filtering through very fine filter.

So the salts you are working with are citrates (in other words did you use lemon in making the tea)?

What precipitated looked like "rubbery"/"Plastic" so do you think that this is what it could have made the original resin unworkable in anhydrous acetone? I meanmany people report that the resin does not dissolve easily in acetone. I am wondering ,you mentioned washing the acetone-washed resin in acetone then IPA then MEK. Was the resin totally insoluble in them? was it difficult to dissolve it in them? If it was not then one could think of doing the acetone step first to remove the lets-call-it-for-now cellulose that makes the resin unworkable, THEN convert it to HCl for and then work it with anhydrous acetone and IPA to get the alkaloids that will precipitate.

Also, i think saccharides in general are SOLUBLE in alcohols.

Have you played with solvent temperatures? That could be interesting as well.

 

[Infundibulum]

The white goo after the addition of acetone in the cactus tea looks like precipitated proteins and/or nucleic acids. It is a very common practise to precipitate proteins using acetone in biology.

How much did the white goo weighted?

 

[Crystalito]

Ah Infundibulum,it could well be proteins indeed, the can precipitate in acetone.From searching around (in other mentions of the method in other places) i think the white substance was around 12 grams ,and the remaining resin 12 grams as well.

 

[soxy bastard]

I have done 6 trials on 50g TBM and each was consistently at 50% by weight this substance.
Question: Is the precipitate actually crystalline or is it a shiny vitreous solid? M/P?
I have never isolated it as you have done, bravo!
SB

 

[Phlux-]

The precipitate is slightly gummy(the white precip) and it does have some taste, just not a whole lot.
The mesc is in hcl form as the resin was picked up and filtered using strong hcl water.
The resin was preddy much insoluble in acetone - ipa broke it up nicely, but didnt change much.
i was thinking alcahols may be the route here - i think that mesc is far more soluble than sugar in alcahols, so using little amounts may work, along with carefull filtering.

 

[Phlux-]

according to the wiki

methanol - Acidity (pKa)15.5
ipa - Acidity (pKa)16.5
acetone - Acidity (pKa)24.2

acetone hardly did a think, ipa semi worked - now methanol is being used.

the resin has become a powder - hopefully the mescaline is in the methanol, and hopefully all the sugars etc is whats left.

 

[Crystalito]

Hmmm sugars might be soluble in methanol, i have been trying to find specific solubility data of saccharides in the net but i cannot.I keep finding though that alcohols dissolve sugars adequately.By the way HERE is a rather interesting article which i have no access to. The abstract is as follows :

Modeling solubilities of sugars in alcohols based on original experimental data

Solubility of six different carbohydrates in methanol, ethanol, 1-propanol, and 2-propanol were measured at 22, 30, and 40°C. Ketose sugars (fructose, tagatose, and lactulose) show higher solubilities than aldoses (glucose, galactose, and lactose). The binary solid-liquid equilibrium data obtained was satisfactory represented by using the A-UNIFAC model. Additionally, the capability of the model to predict the carbohydrate solubility in alcohol-alcohol and alcohol-water mixed solvents was explored.

If anyone has access it could be nice if the article could be provided.

How to remove sugars? Should i go totally crazy here and say "ferment them to alcohol"" Hehehhehehhe....

Hmmm im trying to look over at the details of the procedures and see if we are missing something or if we can tweak it a bit ,hence my preoccupation with details such as temperature and precise questioning on the steps of the procedures, its not OCD :lol:

 

[Phlux-]

well - the methanol wash is doing its trick - there is tan powder and orange transparent methanol - im using just enough to disolve a bit then adding more - i intend to use slightly too little methanol than required to break it all up.
got an idea that seems to be working here - im gona put the methanol in the freezer before evapping to try get more precip out.

 

[Infundibulum]

well - the methanol wash is doing its trick - there is tan powder and orange transparent methanol - im using just enough to disolve a bit then adding more - i intend to use slightly too little methanol than required to break it all up.
got an idea that seems to be working here - im gona put the methanol in the freezer before evapping to try get more precip out.

Phlux, methanol will dissolve both mescaline chloride as well as sugars at various degrees. I believe that your approach will be troublesome due to this fact. SWIM tried to do something very similar in the past trying to separate psilocybin and sugars from crude mushroom extracts.

We however know that sugars are not soluble/hardly soluble in acetone. This can be used to our advantage if one had an acetone-soluble salt of mescaline. Mescaline acetate, fumarate and citrate are soluble in acetone.

 

[Phlux-]

well - there is a massive amount of stuff not being disolved by the methanol - it broke down into powder, the methanol has been separated and is evaporating.
Thanks for the tips inf - i think changing salt type may be the answer.

 

[Crystalito]

Yup,while we may avoid the Non-Polar use, i think as a "tradeoff" we might have to do a little acid-salt playing.If some nice results emerge ,i would propose to recap the method from the start into a viable "standard step" tek.

I am thinking of if citric acid can be used as a first acid in the cactus extraction "en masse", propably using it pure from the grocery store -lots of lemon juice could do but that would introcduce further sugars and propably unwanted contaminations-.

 

[Phlux-]

well - washed in methanol - that broke it up nicely.

this is now going to be tried with a cactus without a massive amount of sedating alkaloids.