| San Pedro Alkaloid Extraction For Dummies, v1.2 |
| Written by Murple | |
| Thursday, 24 January 2002 | |
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Introduction ============ As far as equipment, you will need at least large stainless steel pot, a pyrex baking pan, a large glass jar with a lid, some sort of straining cloth, and a good sized (1 liter) pyrex measuring cup. You will also need some kind of layer separator. A separatory funnel woul be ideal; you can make do with a turkey baster, eye dropper, or glass pipette, but these will take much more work. It may be possible to bypass the need for a separatory device by taking advantage of the freezing points of xylene and water (see discussion under step 2). A supply of pH papers is essential. Do not use any plastic equipment for any steps involving the use of xylene, as the xylene will most likely extract some of the plastic. This could result in having undesirable plastic byproducts in the final extract, with unknown safety implications. If you are using a separatory funnel, drain out the bottom aqueous layer and throw away the top two layers. Alternatively, use a turkey baster to siphon off the top two layers and discard them. (Make sure you dispose of all solvents safely! Do not flush it down the toilet if you have a septic tank. If pouring it down a sewer-connecting drain, make sure to wash it down with large amounts of water.) You will likely find that the turkey baster only gets off most of the solvent and fat layers. To get the thin layer that the turkey baster can't get, try this trick. Siphon off all of the remaining solvent and fat layers, as well as some of the top of the aqueous layer. Put this liquid into a tall thin glass container (a graduated cylinder or test tube, for example), and let it separate back into layers. Then, use an eye dropper to get off the solvent and fat layers, then add the remaining aqueous solution back to the main jar. There is one other possibile approach to separating the layers. Because xylene freezes at -47.7 degrees Celsius, a separation can be done in the freezer. Put the container in the freezer and let it sit for a few hours until the water has frozen solid. The xylene can then be poured off and discarded. I do not know if this will work for defatting, as I do not know the freezing point of cactus fats. If the fats freeze at freezer temperatures, it may not be possible to pour them off with the xylene. This freezing technique can certainly be used later on in steps 4 and 5 to separate the xylene and water layers, however. Repeat the de-fatting process two more times, or until you no longer get a fatty layer after separation. Make sure that you have good ventilation through the whole de-fatting process (or any time you are working with xylene). If you begin to feel light-headed or nauseous, or get a headache, go outside immediately and breathe fresh air until you feel better. Also, make sure there are no open flames or sparks as xylene is quite flammable. 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. 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. 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. 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. "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."
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