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Psilocybe Cubensis Extraction Options
 
zakara
#1 Posted : 2/14/2015 3:19:56 PM

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Report on P. Cubensis extraction:


Reagents:

Ammonia 25% AnalaR NORMAPUR / VWR Chemicals / Batch: 14E200513

Methanol 99,99% gradient HPLC grade / Scharlau Chemie

Chloroform 99,9% extra pure, stabilized with 150ppm amylene / Scharlau Chemie / Batch: 12161306

Isopropanol 99,9% Analysis grade / Scharlau Chemie


Apparatus:

Stuart Heat-Stir magnetic stirrer + stirbar

500ml 3-necked RBF with thermometer adapter + thermometer

Liebig condenser

Aspirator

2000ml Buchner filter flask + funnel

Heating Mantle

500ml beaker


1. 20 grams of dry P. Cubensis were ground to a powder in a coffee grinder and poured into the 500ml beaker, to which was added 200ml methanol with 10ml 25% ammonium hydroxide.
2. The beaker was equipped with a stirbar and set on the magnetic stirrer, the temperature was set to 45 degrees C.
3. The mushrooms were stirred for 30 minutes at 45C and the methanol removed via vacuum filtration.
4. The mushroom slurry was returned to the beaker, 150ml methanol was added and stirring was continued at 45C for 30 minutes.
5. The methanol was again filtered off and step 4. repeated once more.
6. The methanol extracts were pooled into the RBF and the methanol was distilled off under reduced pressure, solvent boiled off at 50C.
7. The residue was washed with 3x 50ml chloroform (a lot of color dissolved into the chloroform and the residue became much paler in color.)
8. The residue was washed with 3x 50ml isopropanol (further coloration and goo dissolved).
9. The residue was washed with 3x 50ml chloroform:isopropanol 1:1 to get rid of further impurities.
10. The residue was taken up in 100ml methanol which was evaporated to dryness under reduced pressure to yield greyish-white semi-crystalline susbstance with a slight yellow tinge.
11. The remaining extract (all of it, from the 20g of cubensis) was encapsulated in gelcaps by the researcher and ingested, who proceeded to trip fucking balls. He had his first reality check at T+ 4:00 hours, when he also had to administer the 'are the pants dry' test. The test came back positive to the researchers' delight.
At one point the researcher was honestly not sure whether or not his pants were wet or dry, which told him he was in a good place. Very happy
12. The researched felt return to baseline at T+ 11:00 hours.

NOTE: the crystalline mass fluoresced under UV light.

ÊDIT: the extract fit nicely into 2x 00-size gelatine capsules.
 

Live plants. Sustainable, ethically sourced, native American owned.
 
Psybin
#2 Posted : 2/14/2015 3:34:44 PM

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How much extract did you end up with? I think it would have been neat to include a little more about the finished product but regardless, a very thorough outline of your tek nonetheless.Thumbs up Welcome to the nexus, we're glad to have you

EDIT: Didn't see the note at the bottom the first read through, my bad. Big grin
 
zakara
#3 Posted : 2/14/2015 3:49:25 PM

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Yeah well i was initially just doing this for my own tripping goodness but the public demanded i post my extraction procedure. Very happy so i obliged. too bad i dont have photos and such, but you see sir, i was a bit off my ass last night.
 
Gone-and-Back
#4 Posted : 2/14/2015 6:59:20 PM
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It's nice to see people messing around with mushroom extractions. Not enough is known about producing super clean extracts. I saw another thread on here a while back that seemed like a really good one too, apparently it was pure enough to vaporize.

It was kinda the same idea, multiple pulls with different solvents that don't dissolve the actives, then a final pull that will yield the goodies. If I ever have enough mushrooms on hand I plan on giving this a try.

Did you add any type of acidic components to the extract before ingesting? I personally would of placed it in a shot glass with lemon juice, let sit for 30 minutes in the fridge, and then take that or suck it up to place into capsules to take immediately.
Everything published by Gone-and-Back are the mad rantings and ravings of a mind who yearns to be free and thinks he knows what he is talking about. However, these are just delusions made to feel that freedom, because that freedom will never come. Any experiments done are purely figments of the imagination, and are falsified to the highest degree. Nothing should be taken seriously from a crazy mans mind.
 
Icon
#5 Posted : 2/14/2015 8:43:11 PM

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Gone-and-Back wrote:
apparently it was pure enough to vaporize.

Rolling eyes

gee the smileys could use some animation. that's an eye-roll
 
zakara
#6 Posted : 2/14/2015 8:46:49 PM

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No acid was used as the methanol was anhydrous and of HPLC grade. I based this tek on hoffman's work, according to him pure MeOH is the single best solvent. I also found mention of use of a slight amount of base, specifically salts of ammmonia. i left the mushrooms soaking in MeOH overnight and upon evaporation there was no residue to be found. Also, based on the bioassay i it worked Very happy
 
benzyme
#7 Posted : 2/14/2015 9:24:46 PM

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Laughing
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
Gone-and-Back
#8 Posted : 2/14/2015 11:44:42 PM
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Icon wrote:
Gone-and-Back wrote:
apparently it was pure enough to vaporize.

Rolling eyes

gee the smileys could use some animation. that's an eye-roll


I will look for the thread and link it, but it's from very well respected members of this board. I believe Benzyme knows the thread, he contributed to it I think.

Everything published by Gone-and-Back are the mad rantings and ravings of a mind who yearns to be free and thinks he knows what he is talking about. However, these are just delusions made to feel that freedom, because that freedom will never come. Any experiments done are purely figments of the imagination, and are falsified to the highest degree. Nothing should be taken seriously from a crazy mans mind.
 
null24
#9 Posted : 2/15/2015 6:55:50 PM

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LMFAO!Laughing
The famous mushroom 'did i piss myself?' stage! Been there, my friend.
Sine experientia nihil sufficienter sciri potest -Roger Bacon
*γνῶθι σεαυτόν*
 
zakara
#10 Posted : 2/15/2015 7:26:36 PM

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Lol i love that test Very happy

EDIT actually i hate that test Very happy
 
zakara
#11 Posted : 2/20/2015 1:49:11 AM

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mods please, could we possibly move this to psilocybin extraction teks or the advanced chemistry bit? ^^
 
Mushroom_J
#12 Posted : 2/20/2015 3:29:12 AM
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I've been looking for something like this.
Well mainly a way to test potency by weight.
Since each trip can vary even at the same dosage, I see the only conclusive way to tell how potent an isolate is, is to do a proper extraction.

My friends dad is a theoretical chemist... I'd feel weird asking him how to go about it. lol.

Any Idea how to extract psilocin without it breaking down?
 
benzyme
#13 Posted : 2/20/2015 4:58:28 AM

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it's definitely not advanced chem, would probably go in the mushrooms forum.

i got identical product just sonicating in methanol, then rotavap.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
MaNoMaNoM
#14 Posted : 2/20/2015 2:34:36 PM

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COOL, i was just wondering last night, how in the mushroom the actives turn blue,
And if you squeeze the stem, you may get a drop of blue water (i havn't tried it)
So i was wondering if it's possible to get a blue extract? it would just be cool.
*ALL WAYS WITH LOVE
 
Psybin
#15 Posted : 2/20/2015 4:34:20 PM

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MaNoMaNoM wrote:
COOL, i was just wondering last night, how in the mushroom the actives turn blue,
And if you squeeze the stem, you may get a drop of blue water (i havn't tried it)
So i was wondering if it's possible to get a blue extract? it would just be cool.


Isn't the blue coloration a result of oxidation of the alkaloids, which would be undesirable? I always thought that was why one is so gentle when harvesting specimens... Wut?

EDIT: Not that it wouldn't be super cool to have a little blue vial of goodies... Big grin
 
zakara
#16 Posted : 2/26/2015 1:51:35 PM

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benzyme wrote:
it's definitely not advanced chem, would probably go in the mushrooms forum.

i got identical product just sonicating in methanol, then rotavap.



thank you benzyme. I agree that its hardly not very advanced. still, looking at the things in the advanced chem bit... oh well. Smile im employed as an organic chemist in a pharmaceuticals company. We are working on and testing some new alzheimers' medication on rats atm.
 
GOD
#17 Posted : 2/26/2015 6:51:39 PM
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If one soaks Cubensis powder in 75 % ethyl alcohol the alcohol turns blue . I've also heard of blue honey .

The reason for the blueing isnt known . Some psilocybe mushrooms like Psilocybe Cyanescens blue at the slightest contact . Others like P .Semilanceata one has to press ...... BUT ...... not all P.Semilanceata bruise blue even if you crush them but one still gets a trip off them .

5 extraction examples that i found that might help ? and / or give some hints and tips . WARNING ...... Its LONG ---- >

1 - This is from Rhodium ---- >

A representative sample of 2 to 10g of dried mushrooms is ground to a fine powder by mortar and pestle. The powder is mixed with 100 mL of dilute acetic acid in a 250-mL beaker. The pH is readjusted to pH 4 with glacial acetic acid. After standing 1 h, the beaker is placed in a boiling water bath for 8 to 10 min or until the internal temperature of the acid mixture reaches 70°C. The beaker is removed and cooled to room temperature under running water. The acid mixture is separated from the mushroom powder by suction filtration using glass wool. The filtrate is brought to pH 8 with concentrated ammonium hydroxide and quickly extracted with two 50-mL portions of diethyl ether. Gentle mixing instead of shaking should be used to prevent an emulsion. The ether is dried over sodium sulfate, filtered, and evaporated under nitrogen with no applied heat.

Crude psilocin will appear as a greenish residue. Recrystallization from chloroform/heptane (1:3) yields white crystals. The resulting powder can then be submitted to infrared and mass spectral analyses.


2 - From A.Shulgin ---- >

There is a fascinating report in the literature that gives a quantitative measurement of the efficiency of extraction of both psilocybin and psilocin from the mushroom Psilocybe bohemica. The citation to the article is Kysilka, R. and Wurst, M., Planta Med. Vol. 56 pp. 327-328 (1990). These Czechoslovakian scientists studied the efficiency of both methanol and ethanol as solvents, each containing varying amounts of water. The results were, to me, both unexpected and most provocative.

The isolation of psilocybin seemed to be quite reasonable. This alkaloid is reasonably soluble in boiling water from which it can be nicely crystallized. It is less soluble in boiling methanol, and almost insoluble in boiling ethanol. And the extraction efficiency is optimum with methanol and almost as good with ethanol. With both, the less water present, the better. The compound is, after all, a perfect example of a zwitterion, the internal salt of a phosphoric acid and an amine base.

But the numbers with psilocin are strange. With aqueous ethanol, the optimum extraction was with a 70% ethanol concentration, and the extraction efficiency dropped almost to zero when there was no water present. But methanol was extremely inefficient regardless of the amount of water present in it. These researchers were apparently surprised by these findings, as they explored further and uncovered other clues. Time is a factor. Psilocin is extracted at a much slower rate than is psilocybin because it is contained intracellularly in the plant, and thus slower to be gotten out. They conclude that many of the low psilocin assays of mushrooms are due to this difficulty of getting the alkaloid out of the plant and into the extracting solventt. Using this information they determined that the levels of psilocybin and psilocin are substantially the same in Psilocybe bohemica, in conflict with the published literature values where very small amounts of psilocin were observed.

Efficient extraction apparently requires patience.

3 - From the net ---- >

Crumble and pulverize the dried mycelial material and combine each 100 mgof this material with 10 ml of methanol. Place the flask in a hot waterbath for four hours. Filter the liquids with suction through a filter paperin a buchner funnel with Celite to prevent clogging. Collect and save thefiltrate liquids. Heat the slurry (the mush in the filter paper) two moretimes in methanol as before, filter, and accumulate the liquids of the threeextractions. To be certain that all of the alkaloids have been extracted doa small extraction with a portion of the used slurry and test with Keller'sreagent (glacial acetic acid, ferrous chloride, and concentrated sulfuricacid). If there is a violet indication, alkaloids are still present and further extraction is in order.

In an open beaker evaporate the liquids to total dryness with a hot waterbath or by applying a hair dryer. Be certain that all traces of methanolhave been removed. The remaining residue should contain 25-50 percentpsilocybin/psilocin mixture. Greater purification can be achieved, but wouldrequire other solventts and chromatography equipment and is hardly necessary.

Each 100 grams of dried mycelium should yield about 2 grams of extractedmaterial. This should contain at least 500 mg of psilocybin/psilocin mixedor about fifty 10 mg doses. Theoretically psilocin should have the sameeffect upon the user as psilocybin. The only difference between the two isthat the later has a phosphate bond which disappears immediately afterassimilation in the body. In other words, in the body psilocybin turns intopsilocin. Psilocybin is a fairly stable compound, but psilocin is verysusceptible to oxidization. It is best to keep the extracted material in adry air tight container under refrigeration. A sack of silica-gel can beplaced in the container to capture any moisture that may enter.

4 - From P.Stammets ---- >

"Another method I have seen is to soak crushed mushrooms in 75+% ethanol. AFter two to three days, the roughage can be filtered, leaving a dark-blue elixir that can be decanted accordingly. For every fresh 5 grams of mushrooms, 25-30 milliliters of alcohol is recommended. Psilocybin and psilocin dissolve into this solvent, and the alcohol also acts as a preservative. I really don't have much experience with this technique, but have talked to people who say it is their preferred method.

5 - A LONG one from PF ---- >

ALCOHOL EXTRACTION

1. Acquire quality psilocybe cubensis shrooms harvested before or just as the veils open andcool dried with desiccant. The more shrooms used in the beginning, the more potent the concentration can be when finished. Use at least several grams of dried shroom material to makethe process worthwhile and effective. The shrooms need to be thoroughly dry to allow pulverization. To pulverize the shrooms, put them into a small strong zip lock plastic bag (freezer bag), cover the bag with a magazine (for protection of the bag) and pound it with the rubber heel of a large shoe. Or, powder them in a small canister type coffee bean grinder.

In a heat resistant soaking vessel (pyrex glass), combine the shroom powder with several times its volume with 190 proof ethanol. This is the "slurry". Place the soaking vessel in a pan of boiling water. Raising the soaking vessel off the bottom of the hot water pan is a good idea for preventing serious sticking of the good extracts. The slurry will start to boil. Turn the water boiling pan heat down and let the slurry sit for a few hours at a warm-hot temp. Alcohol boils at a lower temp than water. Watch the temperatures closely. Things can get totally out of hand and ruined very quickly without close attention paid.

While the slurry is still hot, filter it through filter paper. This is probably the most important part. A good filtration will be efficient and will keep most of the shroom material out, making for a clean extraction. A small lab type vacuum pump powered bottle top filtering funnel with filter disk holder makes it all really easy and fast, with little waste. That is why this extraction idea is really only for the fanatics.

Collect and save the filtrate liquids. Heat the slurry (the mush in the filter paper) one or two more times with the 190 proof as before, filter, and accumulate the liquids of the extractions. The photos at the top are of extractions done twice.

Inexpensive dust-pollen masks make excellent filters for the slurry. These are available at hardware, drug and paint stores. They are usually white or tan colored, fit over the nose and mouth and are held on to the face by a rubber band attached to the filter. Fashion the filter over the mouth of a drinking glass. Squeeze the filter and slurry to extract the alcohol. There are many details to deal with, but doing it once reveals them all. Experience is the best teacher. Store the extracted alcohol in a fresh bottle.

EVAPORATION AND CONCENTRATION

Combine the alcohol extracts into a glass. Place a small electric fan near the glass and point the air flow directly down into the glass until the surface of the alcohol ripples. This will speed the evaporation and concentration. The process will take several hours. The more alcohol extract - the longer the evaporation time. As the alcohol evaporates and the level recedes down into the glass, wash the residue that adheres to the inside of the glass back into the solution. Any fumes that are generated will be harmless because the alcohol is a non poisonous drinkable spirit. Keep flames away from the solution - pure alcohol is very flammable.

One can also use heat to evaporate and concentrate the elixir. Use a double boiler type of setup to heat and evaporate off the alcohol to concentrate the elixir.

The concentrated shroom liqueur will have a pungent mushroomy aroma. Also, a white crystalline kind of precipitate will form in the alcohol elixir (see above photo). Store it in small screw cap bottles or vials in the freezer. Alcohol doesn't freeze solid and will remain liquid. PROCURING 190 PROOF ETHYL ALCOHOL ("Everclear" - "Golden Grain" ect) FROM A LIQUOR STORE

First, call a well stocked liquor store and ask if they have 190 proof ethyl alcohol. Full service liquor stores supply hospitals and laboratories with 190 - 200 proof ethyl alcohol.

If a permit is needed, call the state liquor board (usually in the State Capital) and ask for anapplication to get an ethyl alcohol permit. The fee is 5 or 10 dollars. On the application will be a question asking what the use of the alcohol will be. Write what they more or less want to hear. State that the use of the alcohol will be for "non-toxic surface sterilizing plus herb extraction - preservation - tincture - and perfume making" (or something to that effect). The poison warnings on the alcohol bottles and this idiotic red tape are just bureaucratic nonsense that results in the state making a big fat bundle off of the sale.

SUPPLY LIST

* shrooms

* 190 proof ethyl alcohol (GOLDEN GRAIN - EVERCLEAR ect)

* Pyrex glass wide mouth slurry soaking vessel

* funnel and filtering set up - or

* dust-pollen masks

* small desk fan

Here are some important guidlines for right now! There is one thing about magic shrooms that is universal.Anyone that you know that has taken magic shrooms will tellyou one thing, if asked, and that is that the shroomswere were hard on the stomach. They make most peoplesick, at the least, temporarily, and some get very sick.What makes for the sickness, is that these magic shroomsare not easy to digest. It is the stomachs reaction todifficult to digest food that is the sickness. So theygoal would be to elliminate the stomach, or by pass it.These extraction teks can do that. By making the extractvery potent and using good filtration technique, theproduct can be consumed by mouth so that the salivaand the mucous membranes in the mouth do most of the job.So when anything of the extract reached the stomach, it isbasically digested leaving the stomach with nothing to dowhich results in no stomach upset - just the trip. Thisis the greatest idea in magic shroom history. To elliminatethe ugly physical effects is a real godsend. It makesit all totally superb and beyond any known psychedelicin entheogenic quality and potency.

1. Use warm-hot temps when soaking the initial slurry (shroom-alki).Use the hot water bath idea from the Gottlieb tek below. Avoidhot bottomed slurry soak vessels. The good stuff can bake onand stick very easily.

2. A good filter is a must. Lab quality filter paper helps for a cleaner extract (less shroom stuff). The fanatic should get a little bottle top vacuum filtering funnel with a hand squeeze vacuum pump and fine slow flow filteringpapers. (science supply - not cheap - but affordablefor the fanatics - look for the 47 millimeter filtersized set ups - small but perfect for this).

3. When filtering the slurry, do it while it is hot.

4. The crystals when heated in the initial slurry are free basemolecules. In the final liqueur on cool down, the free basemolecules will coalesce and form crystals. It takes a day ortwo for the process to be complete. The smaller the finalamount of liqueur, the easier it is for the molecules to meeteach other and combine. When you get your final magic liqueur,the free base psilocybin will coaslesce and form whitish crystals.At first they might look like whitish glue, but they transform insolution to hard crystals.

5. The final elixir will have a layer of crystalson the bottom of the storage vessel. The freebase Psilocybinmolecules come together fast in the cool alcohol. When it is time for dosage, reheat the crystal liqueurin its storage vessel in a pot of hot water. Boil theliqueur and stir and scrape deposits from the glassas the liqueur boils lightly. Alcohol boils at a lower temperaturethan water. Keep the storage vessel off the bottom of the boiling water pot.Direct heat is very bad for the elixir, making it stick.As the liqueur boils, the crystals will remelt with time. The large particles of the crystals can be crushed with a long needle probe to hurryup the process. When the crystals are gone, administer themagic liqueur while it is HOT. Using a syringe enablesuniformity and accuracy of the doseages. The hot liqueurquickly becomes cloudy on slight cooling. So a hottemp of the liqueur with remelted crystalsis important for accurate dosage administration.Or the crystals can be dried and used as they are!

6. Or, the crystalline extract can be completely dried by placing the elixir container in front ofa small fan to get most of the liquid out. To complete the drying, desiccant is recommended. Place the small vessel of liquid extract into a larger jar with quality desiccant. It takesseveral days to complete drying, but the final crystalline substance is very dry, loose, and canbe weighed and worked with very easily.

7. TEK personalization through experience is what happens to anyonetrying this. DOSAGE and STORAGE Getting crystals is really moot. I think the following schemefor dosing and storage is the only way to go. With this way,one doesn't have to deal with the problems of crystalizationand other things related. Plus, the dry crystals would be much more prone to potency loss if left dry. If they arein an alcohol solution, that would be better for preservation.

As an example, one can start with 20 grams of dried shrooms.After the filtration of the hot slurry, the resultant liqueurshould be put into an evaporation vessel and with a fan blowingair across the mouth of the vessel, the liqueur should be evaportateddown to about 50 milliliters. Then, in a double boiler, heat thesmall amount of liqueur to put the crystals and extract back intoa cloudy solution. Then while it is hot, dispense 10 cc of theliqueur into waiting small storage jars with watertight caps. Eachsmall jar is allowed to cool, the cap is put on and the jar isplaced into the freezer for storage. Then when it is time to trip,the desired jars are removed from the freezer, allowed to warm toroom temps, the lids taken off, a small fan set up blowing airacross the jars mouths and the liquere evaporated off to a manageble"hit". The small jars then become adminstration "spoons" - wherethe entire contents (alcohol - water - and extract) can bepolished off with the tongue.

My most exciting piece of beginner's luck came when I got rid of some cakes that seemed stalled in their development (and/or had really uneven surface colonization) by splitting up and drying the mycelium for use in place of mushroom dust to create the liquer described in the following link:

By letting the resulting liquer continue to dry out, I wound up with amber colored crystals that could be crushed and placed in gel caps. A few hundred milligrams of this extract sent a curious fruend of mine into orbit, and now he's been bugging the shit out of me to butcher ALL of my cakes to concentrate on this extract and forget about trying to grow shrooms. He claims the trips he got were much "cleaner" (whatever that means) and that the stuff certainly tastes better than the shrooms themselves.

As I recall, there were about 6 or 7 jarsthat seemed to have good mycelial development, but colonization was very uneven, or so slow, that I abandoned them to put better jars in my grow chamber. Rather than just tossing out the slow jars, I decided to break them up and try Prof PF's extraction technique. By the way, the alcohol seemed to absorb a lot of water from the air - it no longer smelled of alcohol, and the drying process slowed down a lot just before the amber tar and then the crystals appeared. I used no heat, but kept a large fan blowing on the liquid over a large, shallow cookie sheet. Yielded 3.85 grams of crystals from 8 ounces of mycelium. We'll be getting even more residues out of soaks 2 & 3. You'll note that this residue us lighter in color than residue gleaned from the water soaks. Also, this residue comes out dryer - no intermediate "tar" stage.

Almost any liquid will extract something from the shrooms themselves or the mycelium. Even water will work, producinga brown syrup that can be dried into a sticky tar. Only the acetone was a bust in extracting the magic - but it does extract some other crud that might make it a good pre-wash for more seriousextractions. Recapping the results of the tests using other spirits,99% isopropyl, 151 proof ethyl alcohol, and 99.9% methanol - methanolwas the hands down winner for getting the crystals. Once the pretty white crystals have dried, they can be re-dissolved in grain alcohol for a potent elixer. The crystals tend to absorb water from the air unless they are kept in a heavily dessicated chamber.





I am autism spectum ........ please dont burn me at the stake for being honest .
 
1ce
#18 Posted : 2/26/2015 11:14:39 PM

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zakara wrote:
benzyme wrote:
it's definitely not advanced chem, would probably go in the mushrooms forum.

i got identical product just sonicating in methanol, then rotavap.



thank you benzyme. I agree that its hardly not very advanced. still, looking at the things in the advanced chem bit... oh well. Smile im employed as an organic chemist in a pharmaceuticals company. We are working on and testing some new alzheimers' medication on rats atm.



You should check out the work they're doing with nicotine ane choline Pleased Amazing stuff!
 
 
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