Well, after a big/lazy month long ipa soak on 75g of bridgesii chips, i made a resin. Dissolved that resin in acetic acid/distilled water, filtered and reduced to 200ml.
This was basified with 15g koh, and ~75ml of limo was added. It was shaken, repeated, and left overnight to decant the cloudyish limo. Pulled the limo in the morning and salted with ~8% hcl/distilled water ~28ml 2x. Solution was orange/yellow (water phase, and yielded a decent amount of brown/orange super dirty sanchez resin/goo when evaporated.
This was dried, and washed with anhydrous acetone a few times. The insolubles were dissolved in distilled water, evaporated, and washed again. All acetone washes were kept and evaporated. Nothing unusual here, decent yields i might add (300mg washed first pull).
Now when things got interesting, i took that washing acetone, put it on a hotplate and let it sit/evap until it was a goo. Then i washed this goo with warm heptane, which brought off a murky yellow heptane.
Concentrated koh was then added to the goo, (~700mg koh, ml or two of water), and stirred/left to react for 30m. Then mgso4 was added to give a crumbly paste, still slightly wet.
This was put on the hotplate, and ~10ml of limo was added, it was stirred, and the limo was decanted off ~15m later still warm through a glass pipette w/ a cotton plug at the tip to filter it.
The dark orange/yellow, but transparent limo, was put into a 15ml vial, and ~5ml of dry fasa was added. Precipitation occurred, and a control was done with the same limo/fasa to ensure its not just fumaric acid precipitating, no precipitation on the clean limo/fasa.
So here's what i think, theres alkaloids in bridgesii(torch/pedro too mabey), other than mesc hcl, that are soluble in dry acetone as the hcl salts (all acetone was kept in closed containers with mgso4/naso4, all came from same batch). This was why i wanted to try this in the first place, as i suspected there was actives being lost in the acetone washes from dirty hcl's. Hydroscobic/hard to dry actives. Perhaps the fumarates precipitate very nicely vs. hcl water salting to a goo/washing with acetone.
Either way, after its done crystallizing/decanting overnight, ill decant off the limo and acetone in the morning, then wash these mystery fumarates with dry acetone. Then dissolve in dh20 and evap. If its a solid crystalline bitter, it will confirm my speculations that some hcl alkaloids from cactus are soluble in dry acetone, while the fumarates can be precipitated out of limo/fasa.
If this means more weight/effects full spectrum crystalline alkaloid extracts, then
. Perhaps fumarates are the way to go if you do acetone washes on your hcl salts, and wish for a more full spectrum/thorough extraction of the alkaloids.
Heres a pic of the limo/fasa vial-
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