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Author: Subject: Black Pepper Extraction results!
TriiodideFrog
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[*] posted on 23-1-2021 at 23:05


This extraction reminds me of my piperine extraction! I unfortunately failed as the solution solidified and hardened:(
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Fyndium
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[*] posted on 24-1-2021 at 06:14


What do you mean by hardening?

EDIT: It's not even brown anymore, after 2.2kg of black pepper it's turned bloody red. I presume this is just because of the concentration of all the dissolved stuff, not something that acetone has reacted with, or that could be hazardous?



piperins.jpg - 191kB

When this is done, I'll distill off any acetone, and then I'll add NaOH in MeOH (93 grams calculated from a video, into min 500mL of methanol), filter and precipitate with water.

[Edited on 24-1-2021 by Fyndium]
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Fyndium
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[*] posted on 27-1-2021 at 02:47


Ok, I extracted the result by distilling off acetone and adding 500mL MeOH which into 93g of NaOH was dissolved, stirring 15min. At least part of crystals were forming in that solution, hence that amount was not merely enough to dissolve it all, so I crashed the whole solution into a 5L flask with cold water, and let it stand for several hours at 0C during when conglomerates formed and floated and eventually settled to the bottom, and then I filtered the whole liquid and washed it with water multiple times in the filter, and the clay-like mud was washed away, and coarser material remained, and the pictures followed.

I wonder if the alcohol phase is not even necessary, but I'm not sure what would happen if the stripped liquid were introduced with direct water-NaOH solution, in order to react all other stuff into water soluble form and remain the piperine to be settled and filtered? Piperine dissolved 40mg/L so it can be practically washed with copious amounts of water without risk of losing any measurable amount of product, expecting the NaOH will turn all other into water soluble form.

I don't know how much it weights, as I didn't bother weighting it when wet, but starting from 2220g of black pepper, a yield of ~110g (5%) would be a textbook success. It sits now in CaCl2 desiccator for a few days, and then I plan to dissolve it in hot acetone in order to recrystallize it.

pip-filt.jpg - 106kB pip-dry.jpg - 391kB pip-cry.jpg - 292kB

[Edited on 27-1-2021 by Fyndium]
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