chromatography of psilocybe semilanceata extract (tek)

joe_aldehyde · huxleys associate

i've recently collected 140g of said species, dried them, put them in a blender and extracted them with methanol, then ethanol, each left to stand for about 2 weeks in the dark and occasionally shaken. all solvent was distilled off, and i was left with quite an amount of brown gunk sitting in the distilling flask. i added some acetic acid to get it out and subsequently evaporated the acetic acid on the oven in my kitchen (i breathed some fumes and got my first mushroom trip from that...nice one! i saw the "door" shulgin keeps talking about in *ihkal). while the gunk was sitting in a little flask for some weeks, large psilocybin crystals formed. i wanted to separate them by putting the stuff in a centrifuge but somehow (hehe) acetic acid got in the extract. now i can assure everybody that there neednt be no worries about the stability of psilocybin - some of the extract accidentally poured out and i got some nanolitre on my finger and half an hour i was tripping again Smile

ah btw. psilocin, which is contained in said species in minuscule amounts is easily destroyed (blue decomposition product) upon exposure of the ground plant material to acetone, so if you want it all, don't do that de-fatting step that is mentioned in almost every extraction tek.

a few days ago i did a test TLC which showed that this extract consisted mainly of psilocybin - it gives a purple colour upon spraying the TLC plate with ehrlichs reagent (p-dimethylaminobenzaldehyde/pDMAB in HCl/ethanol).
a good way to crystalline psilocybin will be to reduce the overall volume of what is left of the extract by whatever means you have (rotavap in my case), spread the gunk at your starting lines on several 25x25cm TLC plates (my test run used alugram SIL with UV254 indicator) and put the plates in your improvised chromatography chamber (that tupperware box your mom left in your place from her last visit will do very fine, just make sure the tlc plates stand upright - better still if you have a lid). the solvent system that serves you best is acetic acid (98%...some call it GAA) : n-Butanol : water in the ratio 24:10:10. i had very sharply separated zones on my TLC plates using that. the rF of psilocybin for this solvent system is 0,33 followed by a zone probably contaminated with baeocystin, so you can cut your plates (always do a test spray on a thin cut-off stripe from the plate, though) between rF 0,33 and 0,58. if you don't care about baeocystin or whatever compound might be above rF 0,58, you can cut off at rF 0,62. above that is some compound that turns blue with pDMAB, don't know what that might be. and don't worry about spreading your gunk on the plates, i did it very sluggishly and still my zones were nicely distributed.
after cutting up your TLC plates, scratch off the TLC layer and suspend it in methanol. filter it, evaporate the solvent and tada - guess what these crystals are. if you have a milligram scale, you can do as i will and approach to your next mushroom trip in a scientific way.

"i once took 5.3mg of pure psilocybin and did a comprehensive writeup of my trip" Smile

ah yes in case anyone asks: don't worry about the uv-indicator ending up in your product - it's not separated from the TLC layer in the TLC process by the solvents running up the plates, so it won't come off if you extract the powder.

paranoid · Mon Jun 27, 2005 2:22 am

baeocystin is supposedly fairly active itself, so probably not a problem for most people. Can cause nausea in high amounts though I believe.

Nice write-up BTW. Been dying to one day grow a bunch of zoomers and extract and purify the psilocybin from them. Might even happen soon, although more for the sake of doing it than anything else.