Wanderer
Rising Star
Hello,
SWIM is looking to "streamline" the extraction process with as few solvents and steps as possible, while retaining the quality and yield. He has a sufficient knowledge of organic chemistry, but has yet to "apply" it to something useful.
So SWIM has supplied me with the following schematic of sorts to get input. It seems almost too simple, but everything seems to check out relatively well as far as chemical theory is concerned. Right?
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Simplest Acetone Extract
1. Basify
I've decided to cut out the defatting process due to the low lipid content of MHRB powder, and because the salt precipitation of the alkaloids into their fumaric complexes isolates them from any fat contamination anyways.
So to basify the MHRB, add enough water to a 1:1-1:5 ratio of a water soluble hydroxide salt (NaOH, KOH, CaOH) and powdered MHRB to make a paste (or add a solution of water and a pure alcohol to decrease evaporation time). Wait until the paste is completely dry.
If you cannot find a hydroxide salt to purchase, one can make some by extracting it from wood ash. Wood ash is mostly potassium hydroxide (very slightly less basic than NaOH, but still good enough) with a bit of sodium hydroxide mixed in. The age-old method is to use a big barrel, put straw or dry organic matter at the bottom of the barrel, and pile in the wood ash on top. Then fill in the water and allow it to percolate through the ash. The straw and organic matter should filter out most particulate matter. Draw off the water from the bottom of the barrel. The water is now highly basic. Use this to mix with your MHRB, or dehydrate to leave crystalized hydroxide salts. Other methods call for things like coffee filters or just allowing the ash to settle in solution, so one can draw off the water from the top.
2. Acetone!
Add enough anhydrous acetone to inundate and have excess in the containment vessel (glass only). Wait until the particulate matter settles and decant & filter acetone. The freebase alkaloids have now passed into solution. The solution will probably be cloudy and have impurities at this point.
3. Salt Precipitation
Slowly add Fumaric Acid Saturated Acetone (FASA) dropwise into alkaloid-acetone solution to precipitate out alkaloid salts. Wait until salts have settled and decant remaining acetone solution. Wash salts with additional acetone until any lipids or other impurities are gone.
Convert to freebase using NaCO3 (1:1). Mix salt and base together, add enough water to make paste. Allow to dry. Add acetone to dry mixture to draw off freebase and leave excess NaCO3 and Fumaric Acid. Decant acetone and allow it to evaporate. Freebase alkaloids are left.
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So basically that's it. I figure even if someone were to use something fattier than MHRB, the precipitation of indoles would prevent most other impurities (tannins, lipids, phenols, etc) from being in the final product. Now because the precipitation tends to be non-selective as far as alkaloids are concerned, the resulting product would likely be "jungle spice". But if one were to do a non-polar wash, the desired alkaloids could be obtained.
This process seems so much more easy and safe than using caustic chemicals and dangerous hydrocarbons. Is there any visible downside to any of you?
------
Results of the Above Tek
So if you read through this thread, you'll notice that nothing precipitated out of the final acetone solution. I have ruled out the presence of water (which would keep fumarate precipitates in solution), so the only other reason for the lack of product would be too low of a pH during the basifying stage. For this reason, I have adjusted the above tek to use a more basic hydroxide salt instead of a carbonate. If someone wishes to attempt the new version, feel free to do so. I am going to do rebasify my left over MHRB and do a non-polar pull to verify that the alkaloids are, indeed, still present.
-- Wanderer
SWIM is looking to "streamline" the extraction process with as few solvents and steps as possible, while retaining the quality and yield. He has a sufficient knowledge of organic chemistry, but has yet to "apply" it to something useful.
So SWIM has supplied me with the following schematic of sorts to get input. It seems almost too simple, but everything seems to check out relatively well as far as chemical theory is concerned. Right?
------
Simplest Acetone Extract
1. Basify
I've decided to cut out the defatting process due to the low lipid content of MHRB powder, and because the salt precipitation of the alkaloids into their fumaric complexes isolates them from any fat contamination anyways.
So to basify the MHRB, add enough water to a 1:1-1:5 ratio of a water soluble hydroxide salt (NaOH, KOH, CaOH) and powdered MHRB to make a paste (or add a solution of water and a pure alcohol to decrease evaporation time). Wait until the paste is completely dry.
If you cannot find a hydroxide salt to purchase, one can make some by extracting it from wood ash. Wood ash is mostly potassium hydroxide (very slightly less basic than NaOH, but still good enough) with a bit of sodium hydroxide mixed in. The age-old method is to use a big barrel, put straw or dry organic matter at the bottom of the barrel, and pile in the wood ash on top. Then fill in the water and allow it to percolate through the ash. The straw and organic matter should filter out most particulate matter. Draw off the water from the bottom of the barrel. The water is now highly basic. Use this to mix with your MHRB, or dehydrate to leave crystalized hydroxide salts. Other methods call for things like coffee filters or just allowing the ash to settle in solution, so one can draw off the water from the top.
2. Acetone!
Add enough anhydrous acetone to inundate and have excess in the containment vessel (glass only). Wait until the particulate matter settles and decant & filter acetone. The freebase alkaloids have now passed into solution. The solution will probably be cloudy and have impurities at this point.
3. Salt Precipitation
Slowly add Fumaric Acid Saturated Acetone (FASA) dropwise into alkaloid-acetone solution to precipitate out alkaloid salts. Wait until salts have settled and decant remaining acetone solution. Wash salts with additional acetone until any lipids or other impurities are gone.
Convert to freebase using NaCO3 (1:1). Mix salt and base together, add enough water to make paste. Allow to dry. Add acetone to dry mixture to draw off freebase and leave excess NaCO3 and Fumaric Acid. Decant acetone and allow it to evaporate. Freebase alkaloids are left.
------
So basically that's it. I figure even if someone were to use something fattier than MHRB, the precipitation of indoles would prevent most other impurities (tannins, lipids, phenols, etc) from being in the final product. Now because the precipitation tends to be non-selective as far as alkaloids are concerned, the resulting product would likely be "jungle spice". But if one were to do a non-polar wash, the desired alkaloids could be obtained.
This process seems so much more easy and safe than using caustic chemicals and dangerous hydrocarbons. Is there any visible downside to any of you?
------
Results of the Above Tek
So if you read through this thread, you'll notice that nothing precipitated out of the final acetone solution. I have ruled out the presence of water (which would keep fumarate precipitates in solution), so the only other reason for the lack of product would be too low of a pH during the basifying stage. For this reason, I have adjusted the above tek to use a more basic hydroxide salt instead of a carbonate. If someone wishes to attempt the new version, feel free to do so. I am going to do rebasify my left over MHRB and do a non-polar pull to verify that the alkaloids are, indeed, still present.
-- Wanderer
(Whether this works or not, I like the experimenting spirit, keep trying to think out of the box 
