arts warrior
Rising Star
swim recently tried to do an extraction with mhrb following this tek.
"1) dissolve 5g of citric acid per 100ml acetone
2) take the shredded/powdered bark and cover it with enough citric acid acetone. Incubate in a warm place, gently agitating every so often. After 2-3 hours, filter off the citric-acid saturated acetone extract and set aside (this solution should have acquired the dark reddish colour of MHRB). Repeat 2 more times.
3) saturate acetone with fumaric acid. Acetone can hold ~20mg/ml fumaric acid if let for a day or so to completely dissolve.
4) Add the fumaric acid-saturated acetone in the citric acid-saturated acetone MHRB extract. One cannot put too much.
5) Set it aside and wait for 2-3 days. One should see a yellowish precipitate on the bottom.
NOTE: In step 2 one is making an acetone extraction and at the same time converting the alkaloids their citrate salt. After addition of the fumaric acid-saturated acetone in step 4, there is an interconversion of alkaloid-citrate to alkaloid-fumarate salt, like:
dmt-citrate + fumaric acid <-> dmt-fumarate + citric acid
citric acid has a pKa of 3.13, while fumaric acid's pka is 3.43. Fumaric acid is a weaker acid and thus in the above reaction one should have most of the dmt as a citrate salt and just a tiny amount as a fumarate salt. dmt-fumarate however is totally insoluble in acetone (while dmt-citrate is perfectly soluble), and it precipitates as soon as it forms. The insolubility of dmt-fumarate acts therefore as a "sink" and given time all of the dmt-citrate will eventually convert to dmt-fumarate and precipitate out.
6) wash the precipitated fumarate salts with acetone, then take them out and let them dry.
7) dissolve the alkaloid-fumarate salts in 5ml of tap water, then and then add saturated sodium carbonate to make the solution basic. The alkaloids will be freebased and the solution will become milky. In 3 days they will precipitate out forming nice needle-like crystal in the basic solution. At this stage, one can filter the solution (nasty procedure since the crystals tend to be sticky and waxy) and retrieve any left alkaloids by dissolving them in acetone.
8 ) Let the crystals dry, wash them with acetone (it removes any traces of sodium corbonate which is totally insoluble in acetone), evaporate the acetone and enjoy the product."
anyway swim did everything according to the tek however when swim added the FASA to citrate saturated mhrb extract nothing seemed to happen, even after over four days no percipitate was seen. is there any way to salvage the product? please help.
"1) dissolve 5g of citric acid per 100ml acetone
2) take the shredded/powdered bark and cover it with enough citric acid acetone. Incubate in a warm place, gently agitating every so often. After 2-3 hours, filter off the citric-acid saturated acetone extract and set aside (this solution should have acquired the dark reddish colour of MHRB). Repeat 2 more times.
3) saturate acetone with fumaric acid. Acetone can hold ~20mg/ml fumaric acid if let for a day or so to completely dissolve.
4) Add the fumaric acid-saturated acetone in the citric acid-saturated acetone MHRB extract. One cannot put too much.
5) Set it aside and wait for 2-3 days. One should see a yellowish precipitate on the bottom.
NOTE: In step 2 one is making an acetone extraction and at the same time converting the alkaloids their citrate salt. After addition of the fumaric acid-saturated acetone in step 4, there is an interconversion of alkaloid-citrate to alkaloid-fumarate salt, like:
dmt-citrate + fumaric acid <-> dmt-fumarate + citric acid
citric acid has a pKa of 3.13, while fumaric acid's pka is 3.43. Fumaric acid is a weaker acid and thus in the above reaction one should have most of the dmt as a citrate salt and just a tiny amount as a fumarate salt. dmt-fumarate however is totally insoluble in acetone (while dmt-citrate is perfectly soluble), and it precipitates as soon as it forms. The insolubility of dmt-fumarate acts therefore as a "sink" and given time all of the dmt-citrate will eventually convert to dmt-fumarate and precipitate out.
6) wash the precipitated fumarate salts with acetone, then take them out and let them dry.
7) dissolve the alkaloid-fumarate salts in 5ml of tap water, then and then add saturated sodium carbonate to make the solution basic. The alkaloids will be freebased and the solution will become milky. In 3 days they will precipitate out forming nice needle-like crystal in the basic solution. At this stage, one can filter the solution (nasty procedure since the crystals tend to be sticky and waxy) and retrieve any left alkaloids by dissolving them in acetone.
8 ) Let the crystals dry, wash them with acetone (it removes any traces of sodium corbonate which is totally insoluble in acetone), evaporate the acetone and enjoy the product."
anyway swim did everything according to the tek however when swim added the FASA to citrate saturated mhrb extract nothing seemed to happen, even after over four days no percipitate was seen. is there any way to salvage the product? please help.
