Mescaline Extractions


Nan's Nook : Archives : Botanicals : Cactus : Mescaline Extractions
Posted by: Fungusmaximus Jun 25 03, 10:11 PM GMT
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Acid-Base Extraction of Mescaline from San Pedro
by Prdy2GO and starlight, HTML by metanoid
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Prdy2GO:

Step 1: Aqueous Extraction

First, you need to prepare a "tea" from your cacti. If using dried cactus, powder it. If using fresh cactus, chop it to small pieces and then puree it in a blender. At this point, it is a good idea to weigh your cactus and record the weight. This will be helpful further on in the process. Put the cactus in your stainless steel pot and cover with just enough water to make a soup. Add some acid to make the pH of the soup fairly acidic. If using citric acid, you want to add about 3 grams per liter of water. Boil the cactus about 20 minutes. If you use sufficiently acidic water, there is no need to boil longer than this. After boiling, strain out the cactus chunks (the marc) and save the liquid. You want to do three acidic water extractions on the cactus. Combine the 3 liquids and toss the marc on your compost pile or dispose of it in some other non-wasteful manner. If the volume of liquid you have is large, you may want to boil it down to a more manageable quantity.

Step 2: De-Fatting

Once cooled, the next step is to de-fat the solution. This step will remove the fats and many other non-alkaloidal plant matter. Make sure the solution is acidic (pH 4 is good) before doing this. If the solution is acidic, the alkaloids will be in a salt form which is soluble in water but not in xylene. Pour the solution into a glass jar (or separatory funnel, if available). Add 25-50% of the solution volume in xylene. For example, if you have 200ml of solution, add 50-100ml of xylene. Put the lid on the jar and gently turn the jar over 50 to 100 times. Do not shake the mixture vigorously as this could result in emulsions that will be difficult to separate. (If you do end up with an emulsion layer, which looks like a thin layer of poorly separated bubbles, bathing the jar in hot water can help separate the emulsion. If the emulsion layer is thin enough, you may wish to just discard it rather than taking the time to let it separate.) Once mixed, let the jar sit and separate out into the different layers. When this is done, you will have a top layer of solvent, a middle fatty layer, and a bottom layer containing the acidic aqueous solution (and the alkaloids).

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 possible 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.

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

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

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 exercise 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."


References

[1]Fletch. Private e-mail. December 7, 2001.

[2]Shulgin, Alexander. Private e-mail. November 24, 2001.

[3]Trout, K. "Sacred Cacti." Second edition, 1999: Chapters 4, 6 and 10.

[4]Trout, K. Private e-mail. December 1, 2001.


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Starlight:

crystallization using sulfuric acid

Just replace steps 5 and 6 above with the step below:

This method relies on the low solubility of mescaline sulfate in very cold water.

(this is not tested from personal experience, but sourced from Trout: Sacred Cacti and Selected Succulents, 1997)

Step 5: Salt Formation and Crystallization

Once you have separated the organic solvent, dark (or in the case of recrystallization at least yellow) with alkaloid and impurities from the basic solution, extract it with dilute sulfuric acid. Use only as much as is required to neutralize the alkaloid bases. A little excess at this point is not desirable, but not of concern. Separate the small volume of aqueous solution now containing the mescaline sulfate and other alkaloid sulfates.

It will need gentle heat to reduce it somewhat, but do not let it become thick, or overheat. Take this solution while warm and insulate it well (a small styrofoam shipping box will work as will being carefully wrapped in towels). Stick the whole thing in your refrigerator until quite cold (near 0C) but do not freeze.

The object is to retard the rate of cooling to as slow as possible. This will cause the formation of large, beautiful crystals. If you chill rapidly a crystalline mush of many tiny crystals will form, trapping impurities.

Take the mother liquor containing the crystals and pour through a buchner funnel. Allow the air to keep sucking through the crystals. Briefly squirt a bit of ice cold water through the crystals to rinse them of any remaining solution. Turn off the air flow briefly and immediately dump out the mother liquor and ice water rinsing and save.

Rapidly resume air flowing through the Buchner. Then quickly rinse the crystals with a little acetone to remove the remaining water. Let the air keep flowing to pull off as much liquid as possible. (If one has access to a cold room all of this will be more efficient).

Take the filter and immediately dry in a warm oven (120-120F) with the door open. Package as soon as dry and keep away from light, heat, moisture, air.

Second and third crops of crystals may be obtained by reducing the mother liquor further (do not allow to become thick) and again chilled. By the third or fourth time other alkaloids will begin to crystallize. These may be grey in colour and have a plate-like structure. They should be easily distinguishable from the beautiful yellow or white needles and prisms of mescaline sulfate.

The sulfate salt can be converted to the hydrochloride salt by acid base and evaporation if so required.

Posted by: Fungusmaximus Jun 25 03, 10:12 PM GMT
EXTRACTION OF CACTUS ALKALOIDS


Fresh cacti, w/ a water content of 90-95%, are difficult to handle; the juice is not easily separated from the fibers, and the presence of mucilaginous substances causes trouble during extraction. Thus, it is preferable to dry the plants immediately after they are collected, in order to avoid losses and deterioration. The plants should be cleaned, the spines extracted with nippers, and the remaining material cut in thin slices and dried in the sun or better in a low-temperature drier (40-60oC). The dried substance is easy to grind, and the powder can be stored if necessary.


The powdered material (10kg) was exhaustively extracted in a percolator with hot, acidulated [0.3% acetic acid] 96% ethanol, the extract filtered and concentrated in vacuo to 500 mL. water was added (2.5L) and concentrated again to 2.3L. The solution was filtered to separate oils, resins, chlorophyll, etc and washed twice w/500mL of chloroform. The aqueous solution was neutralized with solid potassium carbonate, and an excess of 20g was added. A precipitate containing only calcium carbonate was eliminated, and the solution extracted four times with the same volume of cholorform (2.3L). The combined [chloroform] extracts, after having been dried [allowed to stand over] with anhydrous sodium sulfate were concentrated to 780mL and filtered. The solution was extracted twice with 150 mL of 3% aqueous HCl and once with 100 mL water. The aqueous solution was washed with ether repeatedly and filtered. This is the purified aqueous solution of total alkaloids. [This would be a good place to slowly evaporate the water and consume the residue, for further purification of the alkaloids, see below...By the time all the water is removed, there should be no excess HCl around.]

This soln. is alkalinized again with dry potassium carbonate an extracted 5 times with 500 mL of ether. This extract, containing the ether soluble alkaloids, was concentrated to 500 mL. this is A (trichocereine) [this is mostly the more lipid soluble, inactive, dimethyl-mescaline, aka trichocercine]

The aqueous solution [still basic] is extracted three times with 500 mL chloroform, and the extract concentrated to 200 mL; this is soln B (mescaline) [this could be taken to dryness to give mescaline base, probably mostly pure]

Soln B was extracted twice with 40 mL of 5% aq. HCl and once with 20 mL water. The aqueous extract was then washed with 20 mL chloroform and 20 mL ether. After alkalinization with potassium carbonate, the solution was extracted with chloroform and the [chloroform] extract evaporated to dryness. It weighed 4g. After neutralization with alcholic hydrochloric acid, the crude hydrochloride was dissolved in 30 mL. of absolute [ethyl] alcohol and the filtered solution overlaid with 30 mL of ether. The hydrochloride crystallized. re-xtalized from alcohol, the pure salt melted and 181-182oC.

L. Reti Journal of the American Chemical Society, 1951, p 1767


 




Extracting alkaloids from Trichocereus cacti


Instructions for purifying alkaloids from Tricocereus cacti. This is a general method for concentrating alkaloids, with emphasis on mescaline, but which may be adapted to other plants and alkaloids. It requires that the alkaloids be relatively basic and that the base form be less soluble in water. So it would work well for DMT, but not psilocybin or caffeine for example.

The principle of alkaloid purification is to obtain from a plant only that fraction which is basic. This is achieved by a double layer extraction, relying on the principle that amines (as opposed to most of the other compounds in a plant) are soluble in acidic (the salt form) but insoluble in basic (the basic form) aqueous solution. However, the basic form is soluble in non-polar organic solvents whereas the acidic/salt form is not. Thus, by varying the pH, alkaloids can be taken from aqueous solution to organic solution or vice-versa, leaving behind other materials.

Some chemicals and equipment are important for successful extraction of alkaloids from cactus. The chemicals include methanol, dichloromethane or chloroform, sodium hydroxide and hydrochloric acid. The equipment includes a distillation apparatus, a separating funnel, and various beakers and containers, pH tester, and filter. Alternatives can be found for each of these.

Method:

Slice and dry the cactus. I haven't worked out the best way to do this; no matter how I do it, I am always afraid that I am destroying the alkaloids. In general, what seems to work is to slice it thinly, and run hot air over it overnight. The more water which can be removed from the cactus at this stage, the easier the process will be. [Another possibility might be to use a drying agent such as Calcium Chloride see the "Drying and Preservation" section of the Magic Mushroom Growers Guide for more info.]
Pulverize the dried cactus. I have tried using a blender, and it seems to work moderately well. The cactus is tough so you will have to be patient. The finer the grinding, the better the extraction.


Extract dried cactus with methanol. Ideally this is done hot using solvent-extraction apparatus (soxhlet). Various makeshift methods may suffice for a hot extraction, but I have generally merely soaked the stuff for up to a week, cold. Ideally this step should be done three times, and the extracts concentrated. I have done it once for a week, and then washed out the absorbed methanol with fresh methanol once or twice over an hour or two. What you should end up with, after filtering out the bulk of the cactus, is a green methanol extract. Ethanol or acetone could be substituted for methanol, but neither of these is quite as effective. It is generally desirable to use several times the weight of the dried cactus for the methanol extraction, or at least enough to cover it well in a container.


Remove the methanol to leave just an extract residue. This is best done using vacuum distillation, but can be done using atmospheric distillation, to recover the solvent. If you don't mind losing several litres of methanol, you can merely boil the stuff into the atmosphere; just avoid starting a fire. Always no matter what use boiling chips (porcelain) to promote even boiling. Methanol superboils easily, as I have found :-(. Once most of the methanol is removed, you will be left with a hundred ml or so of watery, methanoly, green slime. If it weren't for the methanol and the bad taste, this could be consumed at this point. In general, I would say that it may be worth your while going to the next stage if you can manage it.


Add dilute hydrochloric acid. Sulfuric acid, etc. could be used instead, but I like to use HCl and NaOH, because the product is NaCl, which is of no consequence if it contaminates anything. HCl is not as oxidizing as H2SO4. The HCl should be less than 1M, but not weaker than 0.1M (pH 0-1). Add a few times the reduced volume of liquid - e.g. take the stuff to 400 ml from 100 ml, etc. One good idea is to let the bulk cactus residue (post methanol) dry, and then soak it for a few hours in the acid you are going to use to add at this point. This will extract the last of the alkaloids. Unfortunately, cactus being what it is, will swell enormously, and removing the HCl is tricky. I have resorted to large quantities of HCl and a kind of press to squeeze out the acid from the bulk residue. This acid should then be filtered, and added to the methanol extract residue as above.


(optional) The stuff at this point will be a bit of a mess. Adding activated charcoal and boiling gently for 10 minutes will help to congeal the chlorophyll etc. which is gumming up the stuff. Do not add too much charcoal - less than a gram should be plenty. Too much will absorb alkaloids. Don't use burnt wood, burnt toast, etc - get the proper stuff from the local pharmacist. Performing this step will make the next stages considerably easier.


Filter the HCl extract. This will remove a proportion of the gunge. This will be easier if charcoal was used. The more gunge that can be removed at this stage, the better. Washing the residue with fresh HCl before discarding, and adding this to the rest will ensure no loss of yield.


Carefully basify the HCl solution with NaOH. I tend to use around a 5M solution for this, which is OK as long as you stir as it reacts. Take it well above pH 7. You should get white clouds of alkaloids forming in the solution, and the whole will become turbid as some of the acid soluble components precipitate. Ammonia or KOH should work for this purpose as well. I have had some difficulty with ammonia not being quite basic enough in other systems.


Add dichloromethane (or chloroform); be generous with the quantities if possible. Ideally, one would like to extract into CH2Cl2 3 times with equal volumes, but the amount of solvents gets huge. Ether is not all that good with mescaline extraction, I believe, even though it is easier to separate from water. CH2Cl2 is handy because it has a very low boiling point. It is at this point in the whole operation that the most care and patience is necessary. A separating funnel is really a must - one could plausibly separate the layers with a very tall thin jar and a syringe, but this would be difficult. Ideally, the basic solution and the CH2Cl2 will separate into 2 nice layers, the lower one (organic) containing the alkaloids. Unfortunately, while this is not difficult with most plants, it is very difficult with cactus extracts because the cacti contain so much resinous junk and natural surfactents (to retain water). The best way I have found to separate the layers once you have shaken them together is to add plenty of salt (NaCl) to the water/base layer. This is excellent for breaking the emulsions which form. Be prepared to use large quantities of salt.


Separate dichloromethane layer from mixture and put aside. Repeat steps 9-10 a few times: once is insufficient, three is good, four is excessive. Combine all the dichloromethane extracts together. This should be a slightly green solution. It will contain a bit of water, most likely.


Backwash the dichloromethane once with a solution of salt and NaOH (dilute). This will clean up the last of the junk from the organic solution. Separate the layers as before and discard all aqueous material.


Distill off the dichloromethane (or allow to escape to the atmosphere if you are rich and don't like the ozone layer). I have found that once you are down to maybe 20 ml of residue, the best option is to place the remainder in a petri dish (or some flat dish you are going to store it on) and hitting it with a hairdryer to remove any last CH2Cl2 and water. You should be left with a small quantity of moderately pure alkaloids. This can be easily consumed by dissolving in vodka, e.g., or should be stable for extended periods if refrigerated, frozen, kept airtight and away from moisture. Do not expect more than a 50% yield the first time you try this: theoretically if everything is done properly, the yield should approach 100%, but this is rarely the case.
[This was added later to the post]


I've had a quick scan through that post, and it seems he's been pretty complete in his description. I can add the following information:
 

The initial extraction is very important. You only have as much alkaloid to play with as you extract at this point. Similarly, the more gunk you extract at this stage, the more you'll have to eliminate. Methanol is used because it's not too polar or non-polar, and it penetrates cell walls and membranes quite effectively. Acetone would be as effective, but it seems to pull much more gunk out along with it, and for this reason should probably be avoided. Also note that the better your mechanical mulching process is, the more effective the extraction will be. Also, note that a hot solvent extraction under reflux conditions, or using a soxhlet would be more effective, but bear in mind that some alkaloids may decompose with heat - it's probably worthwhile checking the physical characteristics of the alkaloid in question in your handy Merck index or CRC handbook.


With respect to the degree of acidity and basicity necessary for the extraction, this can only really be found by trial and error. Insufficient difference from neutrality will cause insufficient separation, extremes of pH (particularly too basic) may cause alkaloids to be degraded or other nasty things to happen. Also note that other compounds present may act as buffers - be sure to stir well, and measure the pH using indicator paper or some such.


The final product is a free base. Usually it's unnecessary to go further than this. Forming a salt can be tricky, and would also be wasteful. If you're ingesting the product orally, then it'll salt adequately with the HCl in your stomach. If you're concerned with oxidation by the air, well, use your better judgment (are you really going to wait that long before eating the stuff). Of course, if it's DMT and you're going to smoke it, forming the salt is a waste of time.


Hope that's helpful.


[additionally]


Once you've extracted the goodies into the solvent layer, you attempt to remove any remaining non-alkaloid gunk that may have come along with it. So you wash the extract with basified water, which forms another layer which you discard. Jez describes this in the procedure. It's not always necessary, but once you've got that far, it's usually not difficult to do (i.e. you've got the layers to separate successfully once already)


Posted by: Fungusmaximus Jun 25 03, 10:12 PM GMT
San Pedro Alkaloid Extraction For Dummies, v1.2

by Murple
Introduction ============


This technique is based on information gleaned from K. Trout's canonical cactus tome, "Sacred Cacti," supplemented by suggestions from Alexander Shulgin, and a few real world observations by anonymous researchers. Using this technique, a non-chemist should be able to produce fairly pure alkaloid crystals from San Pedro cacti using common chemicals and household equipment. This technique is designed for simplicity and ease, and will not give the maximum possible yield nor the highest quality results. If you're after every last milligram of alkaloid or you want perfectly pure mescaline crystals, this is not the recipe for you. Of course, if you had the skills and supplies to go for such goals, you probably wouldn't be downloading "how to extract alkaloids" documents from the internet.



Supplies ========


The supplies needed for this extraction are fairly simple to find and quite cheap. In addition to the cacti, you will need xylene (available in the pain stripper department of your local hardware store under brand names such as Xylol). You will need a strong base such as sodium hydroxide. You will need an acid, such as citric acid (available as a pure powder at many grocery stores) or hydrochloric acid (available from hardware stores as a driveway cleaner or muriatic acid), or even vinegar (which is dilute acetic acid). I would recommend using citric acid as it is much safer than hydrochloric acid. While you could probably use tap water, I would highly recommend using distilled water for all procedures.

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.



Step 1: Aqueous Extraction ==========================


First, you need to prepare a "tea" from your cacti. If using dried cactus, powder it. If using fresh cactus, chop it to small pieces and then puree it in a blender. At this point, it is a good idea to weigh your cactus and record the weight. This will be helpful further on in the process. Put the cactus in your stainless steel pot and cover with just enough water to make a soup. Add some acid to make the pH of the soup fairly acidic. If using citric acid, you want to add about 3 grams per liter of water. Boil the cactus about 20 minutes. If you use sufficiently acidic water, there is no need to boil longer than this. After boiling, strain out the cactus chunks (the marc) and save the liquid. You want to do three acidic water extractions on the cactus. Combine the 3 liquids and toss the marc on your compost pile or dispose of it in some other non-wasteful manner. If the volume of liquid you have is large, you may want to boil it down to a more managable quantity.



Step 2: De-Fatting ==================


Once cooled, the next step is to de-fat the solution. This step will remove the fats and many other non-alkaloidal plant matter. Make sure the solution is acidic (pH 4 is good) before doing this. If the solution is acidic, the alkaloids will be in a salt form which is soluble in water but not in xylene. Pour the solution into a glass jar (or separatory funnel, if available). Add 25-50% of the solution volume in xylene. For example, if you have 200ml of solution, add 50-100ml of xylene. Put the lid on the jar and gently turn the jar over 50 to 100 times. Do not shake the mixture vigorously as this could result in emulsions that will be difficult to separate. (If you do end up with an emulsion layer, which looks like a thin layer of poorly separated bubbles, bathing the jar in hot water can help separate the emulsion. If the emulsion layer is thin enough, you may wish to just discard it rather than taking the time to let it separate.) Once mixed, let the jar sit and separate out into the different layers. When this is done, you will have a top layer of solvent, a middle fatty layer, and a bottom layer containing the acidic aqueous solution (and the alkaloids).

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.



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 ================================


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 =====================================


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.



READ DISCLAIMER - THIS ARTICLE IS PLACED HERE AS RESEARCH MATERIAL ONLY. IF YOU USE ANY METHODS DESCRIBED HERE, OR IN OTHER ARTICLES OR POSTS AT EDOT, THEN YOU AGREE THAT YOU ARE DOING SO AT YOUR OWN RISK. EDOT WILL NOT BE HELD LIABLE FOR ANYONE ATTEMPTING TO MANUFACTURE OR INGEST ANY
CHEMICAL(S) DESCRIBED BY THESE PROCESSES.
Other than that, have fun and be careful.

Posted by: Fungusmaximus Jun 25 03, 10:14 PM GMT




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Extracting Pure Mescaline From Peyote or San Pedro Cactus From the Book: PEYOTE & Other Psychoactive Cacti by Adam Gottlieb 1977 Kistone Press Typed and Uploaded by Elric of Imrryr For more interesting and educational files call: Lunatic Labs UnLimited BBS 213-655-0691 1200/2400 ----------------------------------------------------------------

The isolation of mescaline from cacti containing this alkaloid is not difficult to perform and is perhaps one of the most rewarding alchemical processes that one can attempt. The chemicals required for this process are readily available and their purchase arouses no suspicion or interest on the part of government agencies [This may no longer be true, use reasonable caution when purchasing any chemicals - EoI]. The equipment employed is not expensive or particularly complicated or can be constructed very easily from ordinary household items. The entire process can be carried out in any kitchen in a matter of hours by following the instruction below and in the final stages one can verify the success of the procedure by actually watching the crystals of mescaline precipitate in the solution.


One kilo (2.2 lbs.) of dried peyote buttons may yield between 10 and 60 grams of pure white needle crystals of mescaline depending upon the potency of the plants used. On the average the yield is about 20 grams. The usual underground price for a kilo of dried peyote ranges between $125 and $250 (25 to 50 per button). From Indians in the southwestern USA the price is closer to $50 (10 per button). The street price for a gram of pure mescaline is $20 to $30 - if one is lucky enough to find it. One can obtain from a kilo of peyote $200 to $1200 worth of mescaline. If San Pedro is employed one may anticipate a yield of 3 to 12 grams of mescaline per kilo of dried cactus. One can legally purchase a kilo of dried San Pedro for $5 to $10 and from it extract $60 to $250 worth of mescaline. [Note from Elric: The above prices are in 1977 dollars. Neither peyote or mescaline are commonly available these days, but San Pedro cactus is still legally available in most cactus stores.]


PROCESS [NOTE!! In NO CASE should any aluminum cookware, containers, or utensiles be used at any point in the process. Stainless Steel is the best bet.] Grind a kilo of the cactus, place this in a large pressure cooker, cover with distilled water and boil for 30 minutes. Strain the liquids and save them. Return the pulp to the pot add more water and boil again for 30 minutes. Strain the liquids and combine with the first strainings. Repeat this process about five times or until the pulp no longer has a bitter taste. Discard the pulp and reduce the volume of the combined strainings by boiling in an open pot. Do not use aluminum ware.


When the liquids have been concentrated to the thickness of cream (about 1 quart) stop the boiling and stir in 400 g of sodium hydroxide [Carefully and slowly, it will react with the liquid]. This makes the mescaline more soluble in benzene and less soluble in water. If a large separatory funnel is available pour the liquids into it and add to this 1600 ml of benzene [Carefully again]. Shake the funnel well for 5 minutes and let stand for 2 hours. If a separatory funnel is not available the process can be carried out in a one gallon jug with a siphon attached. After standing for 2 hours the water layer will settle to the bottom and the benzene layer will float to the top. Between the two layers will be a thin emulsion layer of mixed water and benzene. Drain off the water and emulsion layers if you are using a separatory funnel or siphon off the benzene layer if you are using the makeshift jug-siphon apparatus. Be certain that neither the water or emulsion layers get into the benzene layer when separating. If any of these layers do get into the benzene during the separation, pour everything back into the separator, let stand and repeat the separation more carefully. It is better to leave some benzene layer in the water and emulsion than to get the water or emulsion in the benzene. Nothing will be wasted. All of the benzene which contains the mescaline will eventually be salvaged.


Sometimes the layers will fail to separate properly. If this is the case immerse the funnel or jug in a deep pot of hot water for two hours. This will break up the emulsion and bring about the separation. Prepare a solution of 2 parts sulfuric acid and 1 part water. (Never add water to the acid or it will splatter; add the acid a little at a time to the water by pouring it down the inside of the graduate or measuring cup containing the water.) Add 25 drops of the acid solution one drop at a time to the benzene extracts. Stopper the jug and shake well for 1 minute. Then let it stand for 5minutes. White streaks of mescaline sulfates should begin to appear in the benzene. If these do not appear, shake the jug more vigorously for two or three minutes and let it settle for another 5 minutes. I have found that when extracting mescaline from San Pedro it is sometimes necessary to shake the mixture more thoroughly and for a longer time to get the mescaline streaks to form. This is probably because of the lower mescaline content in the plant. This would also apply to any peyote that does not have a high mescaline content. After the streaks appear add 25 more drops of the acid solution in the same manner, shake as before and let settle for 10 minutes. More streaks will appear. Add 15 drops of acid, shake and wait about 15 minutes for more streaks to form. Add 10 drops, shake and wait about 30 minutes. Test the solution with wide range pH paper. It should show that the solution is between pH 7.5 and 8. Allow the mescaline sulfate crystals to completely precipitate.


Siphon off as much of the benzene as possible without disturbing the crystals on the bottom of the jug. The next steps are to salvage any mescaline still in the water and emulsion layer. Combine the benzene siphonings with the water/emulsion layer, shake these well together for 5 minutes and let settle for 2 hours as before. Carefully remove the benzene layer, treat it again with acid, precipitate the crystals and siphoned benzene with the watery layer and repeat this again and again until no more crystals precipitate. Siphon off as much benzene as possible without drawing crystals through the siphon.


The next step involves removing the remaining benzene from the crystals. There are two methods to choose from. The first is the quickest, but requires ether, which is dangerous and often difficult to procure. Shake up the crystals with the remaining benzene and pour it into a funnel with filter paper. After the benzene has passed through the filter rinse the jug with 100 ml of ether to salvage any crystals in the jug and pour the ether over the crystals in the filter. After the ether has passed through the filter repeat the rinsing with another 100 ml ether. Then let the crystals dry. If ether is not available or if you do not wish to use such a highly combustible substance, the precipitate and residual benzene can be poured into a beaker. The jug should be rinsed several times with a little benzene and added to the beaker so that no crystals are left behind. The beaker is then placed in a heat bath until all of the benzene has been evaporated.


The next step is to purify the mescaline sulfate crystals. After either of these methods has been carried out dissolve the dry crystals in 200 ml of near-boiling distilled water. Add a pinch of activated charcoal (Norite) and filter while still hot through #2 filter paper. The hot water which contains the mescaline will pass through the filter. The Norite absorbs impurities from the mescaline. After the liquids have passed through the filter pour a little more hot water over the filter to rinse through any remaining mescaline which may have impregnated the filter paper.


Add 10% ammonia solution a few drops at a time to the hot filtrates until the solution registers between pH 6.5 and 7. Place a boiling stone in the solution and reduce its volume to 75 ml by boiling. Remove the boiling stone and allow the solution to cool to room temperature. Place the solution in a freezer or in a refrigerator turned up to the coldest possible temperature and the solution to cool almost to freezing. Tiny white needle like crystals will form around the bottom and sides of the beaker. Break up the crystals with a glass stirring rod while the solution is still ice cold and pour through a filter. Mescaline sulfate is insoluble in near freezing water and will not pass through the filter. Rinse the beaker with fresh ice water and pour this over the filter. The crystals will now be pure white and can be dried under a heat lamp or in an oven at 250 F. More mescaline can be salvaged from the water that has passed through the filter by boiling these liquids down to about 20 ml. adding Norite while hot, filtering through #2 paper as before, chilling the filtrate to near freezing once more, filtering while cold, rinsing with ice water and drying the crystals. This repetition should obtain at least 2 more grams of mescaline sulfate. If large volume mescaline extraction is being conducted it would be worthwhile to repeat this salvaging procedure several more times.


Posted by: ion Jun 25 03, 10:39 PM GMT
3 words:

Not enough filtration.

rolleyes.gif

-ion

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