Ok so swim got a bit of sceletium and decided to try extract the alkaloids but is unsure of the best route to go.

Information gathered so far.


Found at (http://entheogen.ru/ipb/index.php?showtopic=2026)(im not russian - just came across this)

Mesembrine

Monograph Number: 5933
Title: Mesembrine
CAS Registry Number: 24880-43-1
CAS Name: (3aS-cis)-3a-(3,4-Dimethoxyphenyl)octahydro-1-methyl-6H-indol-6-one
Additional Names: 3a-(3,4-dimethoxyphenyl)tetrahydro-1-methyl-6(3aH)-indolinone
Molecular Formula: C17H23NO3
Molecular Weight: 289.37.
Percent Composition: C 70.56%, H 8.01%, N 4.84%, O 16.59%
Properties: Pale yellow oil. bp0.3 186-190°. [a]D20 –55.4° (CH3OH). Freely sol in alcohol, chloroform, acetone; slightly sol in ether. Practically insol in benzene, petr ether, alkalies.
Boiling point: bp0.3 186-190°
Optical Rotation: [a]D20 –55.4° (CH3OH)

Derivative Type: Hydrochloride
Molecular Formula: C17H23NO3.HCl
Molecular Weight: 325.84.
Percent Composition: C 62.66%, H 7.42%, N 4.30%, O 14.73%, Cl 10.88%
Properties: mp 205-206°. [a]D20 –8.4° (CH3OH).
Melting point: mp 205-206°
Optical Rotation: [a]D20 –8.4° (CH3OH)




This info was given to me by a friend :

The following is copied from an MSc thesis from a S.A.'n university.
Pretty standard A-B extraction to obtain mesembrine and other analogues from S. Tortuosum.

They used DCM as the non-polar solvent, but you can replace that with your more readily available / preferred solvent.
Sulfuric can also be substituted with your acid of choice (diluted to 0.05M).

7.1.2 Bulk Alkaloid Extraction Procedure
Plant material (oven-dried at maximum 40 °C) was finely ground using a rotary
beater mill. Approximately 0.5 – 1.5 kg of the ground plant material was weighed
and mixed with enough 0.05 M H2SO4 to cover the dry plant material. After being
mixed thoroughly, it was left standing at room temperature for 1 hour (during
which it was stirred a further two times).
A Büchner funnel was prepared by placing a piece of filter paper (Whatman No. 4)
in the funnel followed by coarse grade celite-577 (enough to create a layer
approximately 2 cm thick). A small amount of acid washed sand was placed on
top of the celite to prevent the celite from floating. The funnel was placed on top
of a 5 L Büchner flask and the aqueous plant material was filtered under vacuum.
The pH of the filtrate was adjusted to 7.00 by adding 25% ammonia solution. The
filtrate was poured into a separating funnel until it was three-quarters full, and
100 ml DCM was added to it. It was shaken well and left to separate into two
layers. The aqueous layer was rinsed three times with DCM, and the organic
layers were collected and pooled.
A cylindrical glass column (60 cm X 5 cm) was plugged with cotton wool, which
was then covered with an approximately 1 cm thick layer of anhydrous sodium
sulphate and packed with coarse grade celite-577 until three-quarters full. A small
amount of acid washed sand was placed on top of the celite to prevent the celite
from floating. The organic extract was then filtered onto the column and allowed
to filter through. The column was rinsed with two to three column volumes of
87
dichloromethane (DCM, CH2Cl2) and the extract was collected in a flask.
Evaporation under vacuum at 60 °C yielded the alkaloid extract. The crude
alkaloid extract was transferred to a pre-weighed screw-top sample bottle, and its
yield was determined.


I think this was from the Corroboree

"Add calcium carbonate. Dry. Smoke. Small quantities may be safe chewed this way as the calcium oxalate is insoluble, but not sure what happens in the stomach, possibly hydrochloric acid will release the oxalic acid."



Anyone with a bit more knowledge in chemistry amped to design some theoretical extraction procedure more suitable to a kitchen chemist ?
Much appreciated.

Its going to be difficult to isolate it on its own but thats not necessary, mesembrine is the dominant alkaloid.

But it is very easy to make crude extracts. If you have dried and processed sceletium you can make a very simple ethanol extract and dry it. Its going to be oily.

The thing with mesembrine and like alkaloids is they always seem to want to stay as oils. You can probably make salts but SWIM has never seen this done before. Defatting with hexane works. DCM works as a good solvent for non polar pull but you can also try other solvents it can't hurt. I bet things like limonene would work.

I guess it depends on the goal. If you want snortable material I've heard you can make solutions with the crude extract. If you want just more concentrated material just do an ethanol extract. If you want smokable material first try the cruder material and see if its necessary to go stronger. I suspect not because smoking sceletium on its own is enough to do something.

its fine to get a mixed alkaloid product and it will always be oily - "Pale yellow oil. bp0.3 186-190°"
perhaps heating it to 150 may knock out some of the other alky's
about the ph - acidic (what like 2?) - defat - neutral ph - extract - then evap ?
what is the pKa of mesembrine ?

Its likely that the other alkaloids are active too so SWIM wouldn't want to try to exclude them. I think heating and exposure to sunlight causes the alkaloids to convert to mesembrine anyway. That's the reason when its traditionally prepared they let it dry out in the sun and do this kind of "fermentation" process. Its not really fermentation but they heat and dry in sun is part of preparation and its been shown that this converts alkaloids to mesembrine.

But anyway I have never seen the pKa reported.

Concerning for acid extract SWIM thinks 3-4 will be fine. (Someone SWIM knows did this once so thats from memory but SWIM can ask again sometime).

defat with hexane will work but so would naptha. non polar pH SWIM can't remember but I don't think it was too high like 13-14 but more like 11-12. Sorry memory isn't too good this was a while back.

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Phlux, Can you please describe the bioassay of this material. I have read about it but havent felt it was worth purchasing. Not enough 'buzz' about it. Is it worthwhile? If so, then why? I am highly curious. It must be pretty good if you are planning on extracting.

Any info appreciated,

J
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idk man - its odd, deffinately not something if ur looking for some kinda buzz.
i usually take a pinch of powder and put it between my gum and cheek, or chew on a pinch if unground - just a tiny pinch is all thats needed.
it seems to give me more energy and clear my mind, mildest euphoria and just a pleasant state of mind.
when too much is taken slight visuals are noted accompanied with discomfort.
im interested in extracting it because i have a whole bunch i got for free and there doesnt seem to be a good tek out there for others potentially interested in playing with this very legal(hehe) plant.

SWIM has smoked and eat sceletium. SWIM likes the feeling it gives. A nice warm stimulating kind of feeling. It helps with concentration and mood for the most part.

There was a report on this website about someone making an ethanol extract i think drying it and then dissolving it some solution to use in a nasal spray. Supposedly it was VERY euphoric. SWIM can't remember where the report is or went but I think someone named lorax or the lorax posted it.

yeah loraxes sceletium nasal spray thread - would still prefer to extract it.

Here are some details SWIM dug up:

Sometimes people in literature defat first (you can probably try both ways).

So defat with hexane 3x.

Make acidic with 0.05 M H2SO4 extract 3x.

Filter and make basic with NH4OH to pH 11. Extract 3x with DCM.


This is of course the procedure that you posted except simplified. This procedure works SWIM knows it does.

I am sure you can change acids and bases. The question would be what non polar solvent to use. You can of course try DCM if its available. Or try other things hexane naptha I don't think will work otherwise the initial defat would be counter productive.

Note that filtering powdered sceletium is a nightmare. Thats why the author of that first paper went through so much trouble with the filtering using sand celite and all that.

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Thanks.

Actually that sounds just about right. I've been delving into stimulating compounds lately. Looking for mental clarity, energy. Sounds great. I'll have to try it soon.


J
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Yea SWIM likes to take it when SWIM has stuff to write it helps SWIM concentrate and stay focused. SWIM also likes to take it if SWIM has been in a bit of a rut then takes sceletium for a few days to boost the mood. Also nice with pot and sex.