Author Topic: dream critique?  (Read 2898 times)

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supernate

  • Guest
dream critique?
« on: May 01, 2003, 11:07:00 PM »
an evaluation of the alkaloid content of Mimosa hostilis root bark.



38g Mimosa Hostilis root bark was pulverized by first scissoring into bitesize kibbles followed by a blendering in 3.145% HCl (w/w). The plant mass was shaken and filtered in 5x 500mL dil. HCl (including the blendering HCl volume)with each acid soak lasting an average of 10hrs. the blood-orange acidic supernates (pun intended) were combined in a clean 4L apple cider jug and washed with 3x100mL napthalene, 100mL toluene (which pulled the most gunk) followed by 100mL acetone (which resolved poorly to give only 30mL of separatable acetone with no gunk pulled). the acidic phase was then bassified with 500mL 8M NaOH to give a dark greyish-burgundy solution with thoeretical pH of 13. 4x250mL dichloromethane were poured overtop, shaken repeatedly and let sit overnight each.

while each basic aqueous phase was sitting with the dcm, the already separated dcm layers were left dirty, sitting in another 4L cider jug ontop of a space heater to reduce the volume to a workable quantity. this mixture, over the course of a few days turned from a clear light amber to a cloudy white, which was a cause for concern.

when the combined dcm extracts were washed with 3x200mL sat. NaHCO3 the cloudiness disappeared with alot of other gunk. the dcm was then washed with 100mL water and poured into a pyrex casserole dish and placed over a space heater to evaporate. this was left overnight to yield a little brown goop in the bottom of the pan, with a few colonies of spiky white crystals here and there in a baking hot pan (oops). while cursing profusely, the contents of the dish were scraped up this morning and shaken in 30mL boiling methanol. the test tube was placed in an ice-water bath in the freezer until it was pretty fucking cold. the orangey-brown supernate was discarded and the ppt. was dried to give .21g sticky light-orange wax which was smeared onto a rolling paper. the alkaloid content of M. hostilis root bark was found to be .55% by wieght.

regrettably, because the chemist has to go into town today for his genetics lab job interview, the product has not yet been qualitatively identified by bioassay. maybe tonight...

so: only .55%, eh? all the resources ive read have claimed .57-1% alkaloids by weight. if only i had a super-large scale gas chromatography machine *sigh*.

what do all you bees think i did wrong, ie, how could i achieve better yields in the future?

N

ClearLight

  • Guest
at least it was only 38 gms...
« Reply #1 on: May 01, 2003, 11:29:00 PM »
Instead of the 100 gms I used... w/ similar results..

 Prior to acidification, use sodium carbonate to remove carboxyl acids....

  Control the ph so it doesn't go to 13 and form a Na Salt..

  try around 10-11 or so..

  After the NaCO3 treatment, run it through some cellite to clean up the potential emulsion gacks..

  These are all things I plan to do after much research into extraction from plant materials etc.. on my next batch.. so i thought i'd add my input here till I can work on that project again ( deep in H2 at the moment lol)


supernate

  • Guest
thx
« Reply #2 on: May 01, 2003, 11:54:00 PM »
verrrry interesting!
thanks, though...
will Na2CO3 remove carboxyl acids? wouldnt bassifying early make your acids soluble in the aqueous phase?
by pulling 2 H+ per mol of Na2CO3, you turn your carboxyls into carboxylate anions, which are very soluble in water.
you remove any acids that make it as far as the dcm extraction with the NaHCO3 washes anyway...
though you could wash the dcm ith Na2CO3 instead, more powerful base, better acid pulling fx...   or TSP (trisodiumphosphate)...
what is cellite? do you use it for column chromatography packing? why not use activated alumina? i just sucked the emilsion gaak up into a pateur pipette: got all the crud out, and didnt lose much goodies as i expect i might by running it all through a column (though it took some manual labour...).

BTW, where do you get your MHRB? i spent a hefty $2/g for mine through some legal outlet downtown. (cleaned out the shelf too!) ive been poking around a few online herbal suppliers which offer much better gram rates...
i am, however, inherently distrustful of online companies.

N

ClearLight

  • Guest
No sources!
« Reply #3 on: May 02, 2003, 03:03:00 AM »
Hmm you haven't been rated yet.. no sources on the hive!

Sorry not to be able to dig up the exact refs on this.. way to busy.. but you have the general idea..

  celite is diatomaceous earth, used for pool filters and chem extractions utsfe for more details..


weedar

  • Guest
well
« Reply #4 on: May 02, 2003, 11:40:00 AM »
there is a link to a ethnobotanical supplier on Rhodium's
site which supplies fairly cheap mimosa.


supernate

  • Guest
!oops
« Reply #5 on: May 02, 2003, 06:48:00 PM »
whoops, 6.022x1023 pardons guys!
no refs no refs no refs no refs no refs no refs no refs no refs no refs no refs.....  ok, i think i got it now.

jeeeeezus, please excuse my abject ameturism!

supernate

  • Guest
qualitative analysis of purity
« Reply #6 on: May 07, 2003, 06:49:00 AM »
the product of said dream was tested for purity by heating in a test tube plugged with a 2hole stopper, one hole acting as an air input, while the other hole acted as an air/fuel mixture (yeah, thats mental fuel) output which was connected to a hose and mouthpiece.
about .05g was vaporized the first time, giving a weak response: auditory and body effects, but without any blood-rushing-in-the-ears or any totally immersive visual effects.
wierd ass talking in my own voice inside my head too. "oog, bloog mig bad booglodoon..." and such. visuals were experienced, but not super-strong: distortion of visual plane -> colored mesh pattern overlay. closed-eye visuals were quite bizzare, though not very vivid.

shit, must be weak-ass shit. i suspect i must have scorched the shit out of the goods when i left the evaporating tray on the heat overnight.

i got fiendish and vaporized the rest. it was a chore sucking all that back (3 loads) but the end was worth it (financially? maybe not.). loud blood-rushing sounds. could 'hear' with the pores in my skin. full vibrating visuals were attained, leading to a 'walk-through' of a series of 'rooms' each with uniquely coulered, patterned walls until a final room was entered, which was a sort of inside-and-outside of the room. as if i was looking at my body from the inside and the outside at the same time.
however, each episode was vanishingly quick. the whole high felt like it lasted 3 minutes, with the residual body stone, not dissimilar to vaporizing weed, lasting another half hour.

next batch SWIS will not bake his shit on the evap dish, and will blast a whole lot more! however, i was dissapointed with the whole thing. it was always made up to be The Ultimate by Shulgin et. al. though i found the high to be too short, and unsatisfying. maybe ill vapo a load of 4-hydroxy-dimethyltryptamine from Psicocybe cubensis instead.

i also wanna try a salvinirorin-A from salvia divinorum using chilled acetone. anyone had success/advice on this dream?