Step 3: Basification
====================
After de-fatting, slowly add sodium hydroxide to the aqueous solution until the pH is up around 10. Rather than adding dry sodium hydroxide, it may be wise to prepare a solution of sodium hydroxide in water, and add this. Be careful when mixing the sodium hydroxide and water, as the mixture will cause an exothermic (heat producing) reaction. Do not prepare the mixture in heat-sensitive containers. When working with sodium hydroxide, remember that it is a highly caustic material and can burn you badly. Avoid contact, especially with the yes, and if any gets on you wash the spot immediately with plenty of water. It is highly recommended that you wear protective gloves and goggles when working with sodium hydroxide or other hazardous chemicals.
Be aware that once you do this step, you need to continue the extraction at least up through the xylene extraction because leaving the alkaloids in a strongly basic solution will cause them to start breaking down after several hours. Making the solution basic turns the alkaloids into their free base forms, which are soluble in xylene.
Step 4: Extraction of Free Bases
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Once the solution is basic, xylene using the same ratio as used during the de-fatting process. Again, mix the solution thoroughly but gently to avoid emulsions. Let the solution sit, and it will separate out into two layers. On the bottom will be a basic aqueous solution, and on the top will be a xylene layer which now contains the alkaloids. Using either a separatory funnel or a siphoning process, collect the xylene layer and set it aside. Since there will still be significant alkaloids in the aqueous layer, repeat this process two more times. Combine all the xylene and discard the remaining aqueous solution.
If you are using a separatory funnel, gas may be formed when adding xylene to the basic solution. To prevent pressure from building up and potentially leading to an explosion, vent the separatory funnel occasionally. If you are using a jar, you should remove the lid.
Step 5: Salt Formation and Extraction
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The next step is to add acidic water to the xylene. This will cause the alkaloids to convert to their salt forms, which are soluble in water but not xylene. If using hydrochloric acid from the hardware store, it will already be diluted and may be usable as is. Read the label to find the concentration. One source says, "HCl from the hardware store is generally between 24%-36% HCl. This is far from dilute. Indeed, upon opening the container, a visible plume of white vapor can be seen creeping out of the bottle. First the lungs start to burn, then any skin which is exposed to the air starts to sting... This should be diluted, especially if it is going to be worked with without a fume hood. 20 drops acid per 500ml of water may even be sufficient."
If using vinegar (acetic acid), it comes quite diluted (around 5%) and should be used as is. It would probably be best to use plain white vinegar. I do not know what else is in vinegar other than water and acetic acid, but it is likely other chemicals remain from the original wine, and this may affect your final product. There should not be any harmful products from using vinegar, since it is a food-safe product, but you may not get nice crystals after evaporation.
If using citric acid (which is the recommended choice), prepare a solution of citric acid powder with a small amount of water. I recommend using citric acid because unlike hydrochloric acid, it is food-safe and safe to handle, and unlike either hydrochloric acid or vinegar, it is available in pure form. I have been told that using hydrochloric or acetic acid has the advantage that both are volatile and that excess will evaporate off, unlike citric acid. However, since neither are easily available in pure form, it is still probably better to use citric acid. Beware that if you do use hydrochloric acid and let it evaporate, the fumes can be hazardous and the evaporation should not be done where you might breathe in the vapors.
For this step, it is useful to have some idea how much alkaloid should be in your cactus extract. If you weighed your cactus before extraction. Trichocereus pachanoi has been analyzed with mescaline contents of 0.025-0.12% fresh weight (0.331-2.0% dry weight). Mescaline is usually around 50% or more of total alkaloid content. You will want to add an equimolar quantity of acid to the solution.
If you can't or don't want to estimate the alkaloid content, Trout gives the following work-around: add very small quantities of acidic water to the xylene, let separate, and then collect the water layer. Check the pH of the water, and it should be neutral. Repeat this with small batches of acidic solution until the water layers come out acidic. Trout points out that "Something to keep in mind is that neutralization won't always be immediate. pH should be checked after a few minutes to see how it is, adjusted if needed and rechecked a few minutes later."
If you are using citric acid and you are not worried about having citric acid powder in the final product, you can just add enough acidic water to make the solution slightly acidic, and repeat this once or twice, then combine the extracted water layers. As citric acid is both food-safe and a solid powder, this is a sloppy but safe approach. Shulgin suggests that this may be a better approach than stopping when the water layers stop coming out neutral: "My gut feeling is that there may be quite a bit of alkaloid still in the xylene, and maybe a couple of extracts with more aqueous acid would be useful. True, it may load the product down with excess citric acid, but the increased yield might be worth it."
However you approach it, after the acidification and water extraction step, discard the xylene. Again, make sure to dispose of it in a safe manner.
Theoretically, this step could be skipped entirely, and you could just let the xylene evaporate. This would leave behind mescaline (and the other alkaloids) in free bas form, which is an oil. This is not recommended however, as mescaline oil is highly caustic and it would burn your skin to touch it. Since its an oil, it would also not be possible to put into capsules. Perhaps you could put the oil into some acidic fruit juice and safely drink it, but it is still preferable to go through this step to produce a salt form. Perhaps it may even be smokable, though I know of no reports of anyone trying to smoke (or vaporize, rather) free base cactus alkaloids. The boiling point for mescaline free base is around 180 degrees Celsius. One final concern is that free base mescaline oil may not have the shelf life of a salt.
Step 6: Evaporation
===================
Finally, pour the water into a large pyrex baking pan. Set it in a protected location to evaporate. Let it evaporate slowly at room temperature rather than using heat, as this will give you a better chance of producing nice crystals. After the water has fully evaporated, scrape up the crystals (or whatever solid mass you end up with) and put them in capsules or a vial for storage.
Keep in mind that when measuring doses, there are a few things to consider. First, your extract will contain all the alkaloids from the cactus, not just the mescaline. Second, depending on what acid you used in step 5, you will have different salts of the alkaloids. For example, if you used citric acid, you will have mescaline citrate (as well as citrate salts of the other alkaloids). If you used vinegar, you will have mescaline acetate. If you used muriatic acid you will have mescaline hydrochloride. The doses of each will be slightly different, due to the different molecular weights of the different acids. Because of these factors, you will need to figure out the potency of your material before you can weigh doses accurately.
Conclusion
==========
Do make sure that you follow all safety instructions religiously. Failure to excersize caution can easily lead to harm and even death. To stress this point even further, I will close with some comments from Trout:
"It seems like it does not matter how many times you tell some people things, lots of them decide what THEY think is really important and items like solvent exposure and not using plastics or solvents stored in plastics (or even the use of slow and careful heating) get forgotten whenever it is not convenient to follow the instructions.
Its very distressing how careless some people are. Worse, people like this often expose not just themselves but family, children and pets with no thought or concern.
You would not believe some of the letters I have gotten. Some of them I almost can't shred fast enough.
I'm sadly coming to believe that a simple citrate tea (lime not lemon) or else dried outer flesh consumed as powder are the only safe approaches the general public is capable of handling responsibly."
Source Materials
================
Fletch. Private e-mail. December 7, 2001.
Shulgin, Alexander. Private e-mail. November 24, 2001.
Trout, K. "Sacred Cacti." Second edition, 1999: Chapters 4, 6 and 10.
Trout, K. Private e-mail. December 1, 2001.