I started another thread where I observed how easy caapi alkaloid extraction is, so I thought I’d describe the process in a bit more detail here:
Preparation of the Brew
In the example shown, I started with 64g of shredded black caapi vine. 1g of fumaric acid was added to the vine. Other acidifying agents may be used, such as about 25ml of vinegar. (Some brews are made without addition of any acid.)
Add about 500ml water to the vine (enough to cover most of it), and gently boil for 30 minutes, covered. Pour off the resultant liquid through a strainer into a larger pot. Repeat this step three more times.
Boil the resultant brew (about one liter) and reduce to a volume of about 400ml. Cool to room temperature (if you want, add ice to speed cooling).
Basification of the Brew
Dissolve 5g of NaOH in 50ml of water. Add this solution to the brew, and periodically stir for about 5 minutes. During this time, the alkaloids begin to aggregate and precipitate. Allow the alkaloids to settle and the solution to clarify.
Remove Soluble Impurities
Siphon off the clear dark-brown liquid and discard.
Add about 200ml water, stir, and allow precipitate to settle again. After 20-30 minutes, the precipitate will have settled, but the solution may still be somewhat cloudy. Rather than wait 12+ hours for everything to settle, siphon off the liquid and save it. Repeat this step two more times.
Acidify, Remove Insoluble Impurities
Add about 50ml vinegar to the precipitate. This will cause the freebase alkaloids to form water-soluble salts, leaving behind insoluble impurities. Dilute with about 150ml water.
Allow solution to settle. When the resultant yellow liquid is nearly crystal clear, remove and save it. Discard the brown sediment. This sediment is mostly bits of plant material.
Freebase the Alkaloid Salts
Add about 5g NaOH to 50ml water. While stirring the yellow alkaloid solution, slowly add NaOH solution. The freebase alkaloids will rapidly come out of solution. Add only enough NaOH to get the alkaloids to freebase – you’ll probably only need 20ml or so of the solution, depending on how much acid you used in the previous step.
Remove Excess NaOH, Salts, Etc.
After most of the precipitate has settled, siphon off the cloudy liquid. Reserve this liquid for an overnight settling.
Add about 200ml water to the precipitate, stir, and allow to settle again. Remove and reserve liquid. Repeat this step one more time.
Before removing the liquid the third time, check its pH. It should be somewhere between 7 and 8. If the solution is still very alkaline, you haven’t removed enough NaOH and must do additional rinses. Repeat until pH is between 7 and 8.
A pH meter or pH test papers are highly recommended, but if you don’t have either, then do at least 4 rinses.
Drying the Freebased Alkaloids
After removing as much water as possible from the freebased alkaloids, transfer the alkaloids to a baking dish or another suitable container with lots of surface area. Allow to dry – under a fan is best. When the alkaloids are dry, they will be noticeably lighter in color. Scrape up the dry alkaloids and store in a cool dark place.
Final Yield
Allow the “rinse” solutions that were collected and put aside to settle for 12 or more hours (in a refrigerator is good). You will be surprised by how much precipitate collects from what were only slightly cloudy solutions.
Siphon off the liquid and discard. Acidify the precipitate, allow to settle, etc. as described above.
From 64g of black caapi vine, the initial extraction yielded 1.068g alkaloids. The second extraction of the reserved liquids yielded another 0.258g. The total yield was 1.326g, or 2.07%
Preparation of the Brew
In the example shown, I started with 64g of shredded black caapi vine. 1g of fumaric acid was added to the vine. Other acidifying agents may be used, such as about 25ml of vinegar. (Some brews are made without addition of any acid.)
Add about 500ml water to the vine (enough to cover most of it), and gently boil for 30 minutes, covered. Pour off the resultant liquid through a strainer into a larger pot. Repeat this step three more times.
Boil the resultant brew (about one liter) and reduce to a volume of about 400ml. Cool to room temperature (if you want, add ice to speed cooling).
Basification of the Brew
Dissolve 5g of NaOH in 50ml of water. Add this solution to the brew, and periodically stir for about 5 minutes. During this time, the alkaloids begin to aggregate and precipitate. Allow the alkaloids to settle and the solution to clarify.
Remove Soluble Impurities
Siphon off the clear dark-brown liquid and discard.
Add about 200ml water, stir, and allow precipitate to settle again. After 20-30 minutes, the precipitate will have settled, but the solution may still be somewhat cloudy. Rather than wait 12+ hours for everything to settle, siphon off the liquid and save it. Repeat this step two more times.
Acidify, Remove Insoluble Impurities
Add about 50ml vinegar to the precipitate. This will cause the freebase alkaloids to form water-soluble salts, leaving behind insoluble impurities. Dilute with about 150ml water.
Allow solution to settle. When the resultant yellow liquid is nearly crystal clear, remove and save it. Discard the brown sediment. This sediment is mostly bits of plant material.
Freebase the Alkaloid Salts
Add about 5g NaOH to 50ml water. While stirring the yellow alkaloid solution, slowly add NaOH solution. The freebase alkaloids will rapidly come out of solution. Add only enough NaOH to get the alkaloids to freebase – you’ll probably only need 20ml or so of the solution, depending on how much acid you used in the previous step.
Remove Excess NaOH, Salts, Etc.
After most of the precipitate has settled, siphon off the cloudy liquid. Reserve this liquid for an overnight settling.
Add about 200ml water to the precipitate, stir, and allow to settle again. Remove and reserve liquid. Repeat this step one more time.
Before removing the liquid the third time, check its pH. It should be somewhere between 7 and 8. If the solution is still very alkaline, you haven’t removed enough NaOH and must do additional rinses. Repeat until pH is between 7 and 8.
A pH meter or pH test papers are highly recommended, but if you don’t have either, then do at least 4 rinses.
Drying the Freebased Alkaloids
After removing as much water as possible from the freebased alkaloids, transfer the alkaloids to a baking dish or another suitable container with lots of surface area. Allow to dry – under a fan is best. When the alkaloids are dry, they will be noticeably lighter in color. Scrape up the dry alkaloids and store in a cool dark place.
Final Yield
Allow the “rinse” solutions that were collected and put aside to settle for 12 or more hours (in a refrigerator is good). You will be surprised by how much precipitate collects from what were only slightly cloudy solutions.
Siphon off the liquid and discard. Acidify the precipitate, allow to settle, etc. as described above.
From 64g of black caapi vine, the initial extraction yielded 1.068g alkaloids. The second extraction of the reserved liquids yielded another 0.258g. The total yield was 1.326g, or 2.07%
