this is not my work but it seems that if you follow some of these procedures and the filter the Psilocybin crystals once they pecipitate from solution you would have fairly pure Psilocybin
here is the link http://www.fanaticus.com/mycoalki.htm



THE CRYSTALS OF THE GODS
(anonymous experimenter who followed the Professors 190 proof extraction TEK)

Suckerfree (Suckerfree)
Posted on Wednesday, August 18, 2004 - 07:26 pm:

March 5, 2003

Psilocybe Mushroom Extractions

Dear Dr. Shulgin:

A friend of mine performed a Soxhlet extraction of 12 grams of powdered Psilocybe cubensis, using 95% ethanol. When the 60 mL of extract cooled to room temperature, many small transparent, colorless crystals had formed on the bottom of the container and did not redissolve on agitation. Do you know what these crystals are? -- Journeyman

Dear Journeyman:

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 solvent. 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.

As to the identity of the crystals that were drifting around in the cooled Soxhlet receiver, from their being insoluble in ethanol, and white, and transparent, I would guess that you are seeing pure psilocybin.

-- Dr. Shulgin
GOTTLIEB

Then, after a little interaction at the web sites, PF found this extraction tek taken from a book by Adam Gottlieb at the EROWID web site.

THE PSILOCYBIN PRODUCERS GUIDE
by Adam Gottlieb 1976

EXTRACTION

Crumble and pulverize the dried mycelial material and combine each 100 mg of this material with 10 ml of methanol. Place the flask in a hot water bath for four hours. Filter the liquids with suction through a filter paper in a buchner funnel with Celite to prevent clogging. Collect and save the filtrate liquids. Heat the slurry (the mush in the filter paper) two more times in methanol as before, filter, and accumulate the liquids of the three extraction's. To be certain that all of the alkaloids have been extracted do a small extraction with a portion of the used slurry and test with Keller's reagent (glacial acetic acid, ferrous chloride, and concentrated sulfuric acid). 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 water bath or by applying a hair dryer. Be certain that all traces of methanol have been removed. The remaining residue should contain 25-50 percent psilocybin/psilocin mixture. Greater purification can be achieved, but would require other solvents and chromatography equipment and is hardly necessary.

Each 100 grams of dried mycelium should yield about 2 grams of extracted material. This should contain at least 500 mg of psilocybin/psilocin mixed or about fifty 10 mg doses. Theoretically psilocin should have the same effect upon the user as psilocybin. The only difference between the two is that the later has a phosphate bond which disappears immediately after assimilation in the body. In other words, in the body psilocybin turns into psilocin. Psilocybin is a fairly stable compound, but psilocin is very susceptible to oxidization. It is best to keep the extracted material in a dry air tight container under refrigeration. A sack of silica-gel can be placed in the container to capture any moisture that may enter.

DOSAGE

The standard dose of psilocybin or psilocin for a 150 lb person is a 6-20 mg dose. We will figure the average dose as 10 mg. The crude alkaloid extraction process given here yields a brownish crystalline powder that is at least 25 percent pure. Each mason jar should contain at least 50 grams of wet mycelium. After drying this would be about 5 grams of material. The crude material extracted from this should contain 25-30 mg of psilocybin/ psilocin or roughly 2-3 hits. This yield may very to some extent depending upon several factors. Many of these species contain less of these alkaloids than dose Psilocybe cubensis and the alkaloidal content of this species may very in different strains. Cultivation conditions have a lot to do with yield too. Higher temperatures (75 degrees F.) cause more rapid growth but lesser psilocybin content than do lower temperatures (70 degrees F.) One must test each new batch of extracted material to determine the proper distribution of dosages. Depending on the potency of the mycelia and how well the extraction was conducted the dose may range between 25 and 100 mg. Also bear in mind that the dose varies for different individuals.
STAMETS

Paul Stamets even mentions extraction in his 1996 book - "PSILOCYBIN MUSHROOMS of the WORLD". Quote - page 50-51 "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. SOme call this "blue juice."
Stamets tek is not very good for several reasons. He says to start with "fresh" shrooms. It is always the best way to first dry the material to be extracted. Water gets in the way of the solvent. "BLUE" is not good either. Bluing is evidence of the magic being broken down or compromised. I think it is the "fresh" material that does that. Dried material does not blue. Bluing is damage and occurs with bruising of the shroom flesh. Stamets again says on page 56 - "...the more the mushrooms are bruised (blued) the less potent they become."

But what is important about the Stamets quotes, is that he knows people that believe extraction is the superior way to go for the magic.
MEDIOCRE RATING FOR CUBENSIS
The only criticism that has ever been directed towards the Psilcobye Cubensis specie is "On the psilometric scale of comparative potency, P.Cubensis gets a rating of "moderately potent," - P. Stamets. That is not the best. And it seems, that potency is the number one goal of all the seekers, accept the new cadre of shroom growers on the web that are more interested in the hobby of mushroom growing than any magic production.

This extraction technique is the answer to the serious seekers of the magic. What PF would recommend is to extract with easy to get liquor store 190 proof ethanol, and make magic shroom liqueurs and elixirs. The advantage of the liqueur is that it is a good way to preserve the magic crystals. Exposing magic crystals to the air is a quick way to breakdown. But in a freezer in an elixir of alcohol, the magic crystals can certainly last a lot longer. This way delivers potency far far beyond any natural magic shroom. When one considers the extract magic in doses of around .1 - .3 gram, no magic shroom can deliver that, unless extracted. So that puts the lowly Psilocybe Cubensis to the top, because of its one really great attribute - THE EASIEST TO GROW - by far.
This technique describes how to extract psilocybin from magic mushrooms with pure 190 proof ethyl alcohol and make a magic mushroom liqueur of concentrated psilocybin to effect a powerful psychedelic dose as potent as desired. The entire process involves only the shrooms and alcohol. The alcohol is untainted with chemicals and poisons because it can be easily acquired from a liquor store (United States) either over the counter (in some states) or with a special permit (most states - see end of article section - "procuring 190 proof ethyl alcohol from a liquor store".
ALCOHOL EXTRACTION OF THE MAGIC CRYSTALS by Professor Fanaticus

SUPPLY LIST

Shrooms
190 proof ethyl alcohol (GOLDEN GRAIN - EVERCLEAR ect)
Pyrex glass wide mouth slurry soaking vessel
Stove top boiling water pot (slurry vessel sits inside) "double boiler"
Funnel, and vacuum filtering set up or Dust-pollen masks
Small desk fan
Stirring tools - spatulas

Acquire quality psilocybe cubensis shrooms (harvested before or just as the veils open and cool 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 make the process worthwhile and effective. The shrooms need to be thoroughly dry (rock hard) 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 Everclear (ethanol). This is the "slurry". Place the slurry steeping vessel in a pan of boiling water. Raising the slurry soaking vessel off the bottom of the hot water pan is a good idea for preventing serious sticking of the extracts. The slurry will start to boil. Turn the water boiling pan heat down and let the slurry simmer and steep for a few hours at a warm-hot temperature. Alcohol boils at a lower temperature than water. Watch the temperatures closely. Things can get totally out of hand and ruined very quickly without close attention paid. Stir the hot mixture periodically and often to keep things loose with no sticking.

After the hot steeping and 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 (clean of shrooms that is - but heavy on psilocybin). A small lab type vacuum pump powered bottle top filtering funnel with filter disk holder makes it all easy and fast, with little waste.

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 extraction's. The photos at the top are of extraction's done twice.

If there is no vacuum filtering device at hand, inexpensive dust-pollen masks make good 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 filtered alcohol extracts into the Pyrex steeping vessel. Place a small electric fan near the vessel and point the air flow directly down into the vessel 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 liqueur. Use a double boiler type of set up to heat and evaporate off the alcohol to concentrate the liqueur. At this point, with hot concentrated liqueur (no crystal precipitate) it is best to go immediately to the storage tek (see Dosage and Storage at the end).

The concentrated shroom liqueur will have a pungent mushroomy aroma (like fungi perfume). Also, a white crystalline kind of precipitate will form in the alcohol liqueur (see above photo) as it cools. Store it in small screw cap bottles or vials in the freezer. Alcohol doesn't freeze solid and will remain liquid.

IMPORTANT GUIDELINES

1. Use warm-hot temps when steeping the initial slurry (shroom-alcohol). Use a double boiler for the slurry vessel. Avoid direct heat to the bottoms of the slurry soaking vessels. The extract has a tendency to bake on and stick very easily.

2. A good filter is a must. Lab quality filter paper helps for a cleaner extract (less shroom stuff). A small bottle top vacuum filtering funnel with a hand squeeze vacuum pump and fine slow flow filtering papers is perfect for this small extraction tek (look for the 47 millimeter filter sized set ups).

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

4. When heated in the initial slurry, the psilocybin alkaloid extracts are free base molecules. In the final liqueur on cool down, the free base molecules will coalesce and form crystals. It takes a day or two for the process to be complete. The less the final amount of liquid is, the easier it is for the free base psilocybin molecules to meet each other and coalesce into the whitish crystalline substance.

5. The crystalline extract can be completely dried by placing the liqueur container in front of a small fan to get most of the liquid out. To complete the drying, desiccant is recommended. Place the small vessel of liqueur into a larger jar with quality desiccant. It takes several days to complete drying. The final crystalline substance can be weighed, worked with and experimented with.

6. TEK personalization through experience is what happens to anyone trying this. Extracting plant material is an ancient art, and the ways are myriad.

DOSAGE and STORAGE

On cooling and with time, the free base psilocybin molecules coalesce in the liqueur and precipitate into a whitish crystalline extract which falls to the bottom of the storage vessel. The freebase Psilocybin molecules come together fast in the cool alcohol.

Storage and dosage prep is the same. If the liqueur has already precipitated the crystals, heat the final concentrated liqueur (for example - 20 grams of dried shrooms can be extracted to 50-100 milliliters alcohol) in its storage vessel in a pot of hot water. Boil the liqueur and stir and scrape deposits from the glass as the liqueur boils lightly. Alcohol boils at a lower temperature than water. Keep the storage vessel off the bottom of the boiling water pot. Direct heat is very bad for the liqueur, making it stick. As the liqueur boils, the crystals and extract will remelt with time. The large particles of the crystals can be crushed with a long needle probe to hurry up the process. When the crystals are dissolved, administer the magic liqueur while it is HOT. Using a syringe enables uniformity and accuracy of the dosages. Keep the liqueur stirred up to keep it uniform. The hot liqueur quickly becomes cloudy (precipitate) on slight cooling. A hot temperature of the liqueur with remelted crystals is important for accurate dosage administration.

While it is hot, dispense equal portions of the liqueur (10cc-20cc) into small storage jars with watertight caps. Each small jar is allowed to cool, the cap is put on and the jar is placed into the freezer for storage. Each jar is equivalent to an exact fraction of the original dry shroom weight so that dosage can be accurately controlled and determined.

When it is time to trip, the desired liqueur jars (with potency ratings) are removed from the freezer, allowed to warm to room temps, the lids taken off, a small fan is set up blowing air across the jars mouths and the liqueur is evaporated off to a manageable "hit" (variable alcohol). The small jars then become administration vessels where the entire contents (alcohol-water-crystalline extract) can easily be completely consumed.

PROCURING 190 PROOF ETHYL ALCOHOL ("Everclear" - "Golden Grain" et) 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 an application 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).

Professor Fanaticus
2005

Super interesting post! thanks for the info!

Have heard of this being done without the filtration and evaporation/concentration processes and the dosage was done by using a simple shot glass worth of the alcoholic mixture. The effects were a potent 8hr journey.

That's not how things work; unfortunately you won't get pure psilocybin crystals with any of these approaches, as people who have performed said procedures already know (for a myriad of reasons that have been discussed extensively elsewhere in the forum).

to the OP, your title is misleading, so please change it.

im saying if you filtered out the crystals it would be pretty damn pure ive talked to people that have done this and ther product was snow white although that does not mean 100% pure its pretty good i mean as you know any simple A/B teks do not yield pure DMT. but im sure if you took the filtered crystals and then maybe even did a reX its going to be pretty pure

Just for the record. I am not the Journeyman refered to in this post. I am new to the psychodelic community.

You seem a bit misguided...
you can't "filter" pure psilocybin from the proteins bound to it, not by the way you're thinking.

In the procedure you listed, it says that psilocybin is isolated as a "free base", That is plain wrong, because psilocybin is never a free base. why? because it always has a charge state on at least one of its functional groups. because of this, it readily binds fungal proteins.

for this reason, it disappoints me that shulgin would suggest that ethanol would yield pure psilocybin. proteins and nucleic acids also precipitate in cold ethanol, ask any molecular biologist.

This could work, however psilocybin oxidizes extremely quick and would lose its potency if im remembering correctly

explain why it could work, and explain what part of the molecule oxidizes, and why.
(hint: you're thinking of psilocin, not psilocybin.)


I've tried this method, I've also tried a/b, several times.
this method is detailed, and effective, but you're looking at 40% alks, tops.
the only wy you're going to separate the alks from the proteins is some form of chromatography, SEC with weak acid/base followed by cation exchange gets my vote.

Bubble already burst I see...

This has been discussed at length many times before, those crystals which precipitate out are, for the most part, inactive. They are most likely to be fungal sugars. I am planning my own extract soon enough, but the only layman's route to a pure (or as close as kitchen chem will allow) psilocybin is achieved another way than simply precipitationg it out of solution (or so far as anyone can come up with). You need to extract it as a crude resin then clean it up with the right solvents.

Shulgin got it wrong. Hard to swallow but it's the the truth.



Psilocybin is stable enough for storage just as DMT freebase is, psilocin is the troublesome one, much to everyone's disappointment.

the sugars aren't so much the problem, although they may participate in H-bonding interactions,
the problem is the proteins (enzymes) which bind electrostatically and through nonspecific interactions (van der waals). this is why simple filtration will not separate them, and why extracts appear greenish.

for all practical purposes, the alcoholic extract is fine for a crude extract, it's effective.
evaporate the alcohol to obtain the actives.

so i guess tour saying shulgin does not know what he is talking about? and for any kitchen chemist producing 50 percent pur psylicibin is pretty damn pure youd have to take lets say 30 mg instead of 10

infact in the article itself it says that it producec 40-50 percent psylocybin so i dont understand why you are saying this doesnt work when infact you said and i quote "this method is detailed, and effective, but you're looking at 40% alks, tops"
i mean the dosage is so small anyway 50 percent purity sounds pretty nice to me

well, its far from almost pure at %30-40. and most would rather not waste at least half their yield using this method imho. not saying I know of a better method, just that personally, it seems impractical, and your getting friction for the claim of almost pure, When in practice its less than 40% pure.

The great Heisenberg would certainly not approve of 40%

benzyme you said you have done an A/B extract on psyilocybin but b4 you wrote that you said that psyilocybin is never in free base form. so how is it that an A/B extract would work?
also this is the easiest rout to achieve FAIRLY pure psylocybin and i doubt people are going to be doing chromatography at home and for that matter why you would NEED 100% pure psylo for your personal use especially if the impuritys are sugers and inert substances. i dont understand why this has raised so much hate when in fact it is easy to do the yield is pretty good and its also pretty pure i did not state in the title 100% pure and if someone were to actually take the time to read the entire thing all of the things people are stating and arguing about are stated in the above information.

also day tripper were are you getting that this is less than 40 percent pure have you done this yourself and analyzed said compound. and were did u get the idea that you are losing half of your yield.

I stand by the fact that i never said this is 100% pure and i also stand that this gives FAIRLY pure psylo for the great Heisenbergs out ther hanging out at web forums i think their time has been seriously wasted

last things mushrooms can have unknown concentrations in them this method ensures the user that you are taking a dose wich you are comfortable with along with the benifit of having less nausea as some people have.

Please do not be so defensive, there is not need for that.

When we talk about 'almost pure', we mean near 100%, like 99.8%. And utmost 40% is nowhere near pure.

On this site we want to post reliable data, and that includes the verification of claims. So even though 40% is nice, it is far from what we would call pure. Remember that even the best professionals can make mistakes or make statements that can be explained is different ways. Lets say that previously we got 10% (just picking a number here) and now 40% then that is relatively a lot purer, we can even say that it is incredibly pure compared to the previous method, but it still is not what we would call 'almost pure'.

So the best way to handle this issue is to change the claim from 'almost pure' to 'up to 40% pure' and all will be settled.

Remember that this is a site where we research entheogens and where we have to support the results with valid data and reliable sources. It also means that you will face peer reviews from knowledgeable members, all to make sure that our data is reliable. If you don't like the outcome of those reviews then don't get angry at the peer reviewers but look at how you can improve your research and if needed how to change your claims to pass the peer reviews.


Kind regards,

The Traveler

you are assuming that the end product of a/b extraction is always freebase.in reality, when performing a/b extraction's the extracted molecule on the end is not always extracted as freebase.

there are cases where the wanted substance is prefered as a salt, many freebase alkaloids are hard to measure or manage in their freebase state.

in the case of psilocybin, you cant freebase the alkaloid with high PH, as benzyme stated. but you can manipulate the Ph carefully to change the polarity of the molecule, and with that you make it more soluble in non polar solvent's.



you are only making your own assumptions. how do YOU know that you get fairly pure psilocybin from this tek ? have tried it your self ? do you have any results to post for comparison. also what is fairly pure for your standards, 30-40 % ?

no one is showing hatred here otherwise, i percieve your attitude as overly defensive over some ideas that are not originally yours. there are people working in labs on this forum that know their job. they are not just assuming stuff.

It won't even be anywhere near 30-40% pure from a simple alcohol extract. You're going to be looking at a sticky resin that behaves kind of like tape when stored with desiccant, kind of like a gummy film which is nowhere near 30-40% psilocybin. You'd be lucky to get that after the full cleanup. It's just bollocks mate.

I'm saying shulgin is human, and even doctors make mistakes.
he stated it was a guess, not a fact.

I know you think you've found the holy grail of musrhoom extraction teks, I once thought it was too.
..but then I started looking at the pKa's of psilocybin, and realized isolating the compound is considerably more complicated than I previously thought.
yes, I've tried the a/b extraction, but on the basic side (pH 8-9), there is a negative charge on the 4-position oxygen. by definition, this is not a free base.
this is also why ether is used to extract it, nonpolars like xylene and toluene do not permit migration of charged particles (they are not miscible with water).

changed title to 25-50% sorry for being defensive i just though that the white transparent crystals that precipitate were fairly pure