|Mescaline Extraction w/pics||4||4/03||Nan|
|Yet Another Version||-|
|Several Good Mescaline Extractions||4||7/03||Fungusmaximus|
|Real Mescaline?||28||02/19 10:08am|
|Caffeine Extraction (PDF file, works for mesc)||-|
|Chat with Camel - Alkaloid Extractions||4||6/03||Camel|
|By Nanook on Monday, October 22, 2001 - 05:14 am:|
Assuming knowledge of the previous posts, pure mescaline sulfate can be
extracted from syrup.
Let three liters of Pedro syrup rest in the fridge for a month or so until all cell fragments have settled out and decant only the clear syrup off in a gallon glass cider bottle. This is the extraction bottle.
Add 3 cans of lye, slowly and gently, into the syrup. Add only about a third of a can at a time, cap the bottle and shake gently. It will heat and expand so loosen the cap after shaking gently to allow pressure to escape.
After the lye is dissolved, add a quart of xylene paint thinner to the extraction bottle, shake violently and let sit 12 hours.
Decant off the xylene into a precipitation bottle. It is best to purchase a wide mouth ground glass one liter bottle for precipation... But the container should be glass with a seal that is not affected by solvent or acid.
Into the xylene in the precip bottle drop in about 10 drops of sulfuric acid. Car battery acid works just fine (just don't get it from a car battery Rolf says). Shake the bottle and it will turn into one of those "winter wonderland" paperweights with crude mescaline sulfate precipating out like a snowfall.
Add a few more drops of acid and shake until no more precipitate falls out of solution. If liquid acid begins to collect on the bottom of the precip bottle the snowfall is over.
Let the precip bottle sit until all precip has settled on the bottom, then decant the xylene back into the extraction bottle. Shake the extraction bottle violently then set aside to rest 12 hours.
Place the precip bottle into a hot water bath in a well ventilated area until all of the xylene is driven off, then add a few mils of hot distilled water and shake to dissolve the crude mescaline and residual acid.
Decant the water solution into a glass storage bottle. The extraction bottle can be worked for about a week before it is exhausted. The storage bottle should end up with several hundred cc's of crude mescaline solution.
Add strong ammonium hydroxide (ammonia) to the storage bottle, drop by drop, and stir. Stop every few drops and test the solution with pH paper. Add ammonia until the pH reaches 7.0
Add a tablespoon of activated charcoal to the storage bottle, heat to steaming, stir, and filter. Use a wash bottle with hot distilled water to rinse down the charcoal. Repeat this 2-3 times until the solution clears.
Boil the solution down to 200 cc. Place the solution in a freezer or a salt-ice water bath. As the temperature reaches 32 degrees in the solution, needles of pure mescaline sulfate crystals will grow out.
The best way to recover these crystals is to freeze a Buchner funnel with a piece of filter paper in the bottom. Place a vacuum source (cheap venturi pump works well) on a vacuum flask, insert the cold funnel, turn on the vacuum, and dump the half frozen mescaline solution onto the filter. The water will be sucked out before the solution warms leaving pure mescaline crystals on the paper. Dry under a heat lamp.
Boil the remaining solution down to 100 cc's and repeat the cold crystallization.
Properly perfomed this extraction yields about 1/4 ounce of mescaline sulfate crystal...
|Posted by: Nanook Nov 22 02, 03:25 PM GMT|
| General Alkaloid Extraction - again courtesy of Zilla
The method I use is a general one - I copied it from one used by some
scientists to extract mescaline from peyote, but I have since seen close
variations used on many plants. This procedure is followed whenever a plant is
studied for its alkaloids. [This article was contributed by a member of the
Entheogen community, but its original author remains unknown.]
A few ingredients and bits of equipment are necessary. I am a chemist, and
have my own chemistry set. I have considered manufacture, but I find that there
are enough interesting things to do just extracting natural compounds, which is
much easier, indeed, possible in the home.
You will need:
A few flasks, glass containers, etc. of suitable sizes, depending on how
large a volume you are playing with.
A separating funnel is almost essential - this could be tricky to get
without a little effort. If you don't know, it is an inverted conical flask with a
hole at the top to pour stuff in, and a tap at the bottom to let the stuff out
accurately. It is used for separating immiscible layers.
A vacuum filtration apparatus would be very useful; I did have a bodgy
one rigged up myself, but it was always difficult to use. Some kind of still,
though, is pretty important to have, although conceivably for a once off
you could get by without it, if you don't mind breathing in a lot of solvent.
As far as a still goes it is to recover solvent, and leave goodness as a residue at
the bottom. I use a bit of quickfit I nicked: a round bottom flask, short column,
thermometer on top, and a small condenser... takes forever, but don't expect to
follow this procedure in anything under a day.
Other bits and pieces:
A filtre of some sort is a necessity; preferably a good one, with a vacuum pump if
you are filtring gluggy stuff (cactus is the worst, sticky goo, e.g., other things like
seeds and bark are better). People have been known to use such devices as
coffee filtres, t-shirts, tins with holes in the bottom (as a filtre press) and so on.
Whatever you can scrounge. A lab buchner funnel, sidearm flask, and venturi
pump are ideal. All this stuff is standard in any chemical lab, regardless of
The paydirt (obviously)
Some solvents: methanol (lots), and a non polar solvent. Some people use
ether - this is dangerous and doesn't dissolve everything. Your best bet is
probably something chlorinated - I use dichloromethane, although
chloroform will do (don't breath too much - it is fun at first, but ends up
making you feel ill). Drycleaning fluid... petrol... I don't know what you have
access to. Dichloromethane is good because it is non-toxic, volatile, and a
good solvent. It has a major drawback: separation is often very difficult once
you have placed your gluggy plant muck in there. The shot is to use large
quantities of everything, and be patient.
You will also need an acid (Hydrogen chloride is good)
and a base/alkali (Sodium hydroxide is good - that way, if you stuff up, you
end up synthesizing salt instead of something nasty.)
Also useful: acid/base indicator paper, boiling chips (porcelain grains) and
activated charcoal - see local chemist.
The idea is this: Most fun compounds (the only exception is maybe THC, and
alcohol if you count that) are basic - they contain nitrogen. So: in general, if you
react them with hydrochloric acid, they form a water soluble chloride. If you react
them with dilute base in the aqueous phase, they go back to being a base, which
is insoluble in water, but soluble in organic non-polar solvents (like CH2Cl2). So,
the theory is, that only a base will go from water to solvent and back to water etc.
when changed from acidic to basic and back to acidic. This gives you a way of
removing all the other crap which is not alkaloid from a sample. That is the theory.
When I do this, if I can get down to some brown or green sludge that I can throw
down or smoke, I am happy with a good days work. Ideally, you should end up with
lovely white crystals, but I think that would require a lot of time and effort, and
indeed a considerable loss of product in the process.
Get your stuff.
Dry it as much as possible - this makes life easier later on. You will never
get all the water out, but too bad.
Chop it up as fine as possible: a blender comes in handy. You may wish to
chop then dry. A word of caution: try to avoid exposing your stuff to excessive
heat. I dry in low heat oven. Heat and air destroy good compounds from
upwards of 100 degs C. All this bit will depend on exactly what you are
Once it is finely divided - powdered if possible, put it in a big container, and
cover it with methanol. Alternatives to methanol here are ethanol (not as
good) and acetone (good solvent - rips the crap out of anything, but is more
reactive - can react with your actives).
Now, depending on what your stuff is, you have to let the methanol have time to
remove it all. This is best done by leaving in a quiet warm place for a few days,
even up to a week, and shaking it occasionally so it is mixed. Some papers
recommend solvent extraction (soxhlet apparatus) and refluxing at the boiling point
of the methanol (80 degs or so - I can't remember). I usually just rely on time to get
the good stuff out. When you are ready (early in the morning), filtre the muck, to give
you methanol+dissolved brown gunk, and a residue soaked with methanol. The
residue still contains a lot of good stuff, so soak again for an hour, and repeat, and
do a third time if you are feeling generous (3 is the magic number in extraction
When you are done, there is another thing you can do finally, if desired: depending
on what your stuff is, mix it up with dilute hydrochloric acid, 1M is appropriate. let
stand for an hour, then filtre (this may be very difficult) That will get the last of the
alkaloids out of the substrate.
You now have a methanol-plant stuff mixture, and a dilute HCL-plant stuff mixture,
if you bothered to do that part.
Evaporate the methanol, to leave a small amount of goo. This will contain water, a
bit of methanol, and all kinds of resins and muck, and if you are lucky, the
If a very quick and crude extraction was all that was desired, then after stripping the
last of the methanol with vacuum if possible, this residue could be smoked, eaten
or whathaveyou. I leave that to your discretion. However, if a cleaner product is
desired, the double layer extraction will need to be performed.
Combine the evaporated methanol gunge with the hydrochloric acid filtrate if you
have any. If you don't then mix the methanol stuff with an excess of dilute (1M) HCl.
Feel free to filtre again at this point. Anything of marginal solubility here is no good
to you. Get the stuff as clean as possible. Boiling with activated charcoal is another
useful trick for removing gunge. Just boil it up, and filter off the charcoal for a
You should now have an acid aqueous solution of alkaloids and water solubles
from the plant.
Take your acidic solution, and basify. This is done by mixing in dilute sodium
hydroxide (I use up to 5M to save on total volume. Be careful with concentrated
NaOH - apart from eating skin, it eats alkaloids) As you mix in the NaOH, you will
see swirls of white precipitate form and redissolve. Continue until the white swirls
stay, and until the solution is quite cloudy. Indicator paper is necessary to see that
the solution is basic. If you can't get indicator paper, you can make an indicator by
boiling up some purple flowers. The dyes in most flowers go bright red in acid,
and green in strong alkali. Just a drop of dye and a drop of mixture should tell you
what is acid or base.
The white precipitate is the alkaloids. The more the better.
Next, add equal volume of non-polar solvent (dichloromethane) to the mix. Place in
separating funnel, and shake. Separate. This may be very difficult or slow. Adding
more solvent, more basic water, etc. may help. Adding lots of salt to the water layer
will help break an emulsion. Ideally you want to do this step 3 times - to extract as
much as possible from the water layer into the organic. I find this part very difficult,
and you have to accept that you will lose quite a lot of material here. It is, however
probably easier with some plants that others: cactus is very difficult, barks and
seeds would be easier. Use plenty of salt, and agitate to separate.
When you have finished extraction, chuck the basic water layer. The solvent layer is
kept, and can be backwashed with salty water for a cleaner mixture.
The solvent can now be dried, (using salt or some dry powder, the filtred) (I don't
usually bother with this - the old hairdryer at the end can remove some last solvent
and water) then strip the solvent in a vacuum to get your final product - some kind
of syrup could be expected. This is super concentrated, but may only be half the
strength of the original. e.g. put in enough for 10 doses of morning glory seeds, get
back 5 doses or more of concentrated alkaloids.
If it is desired to take the process still further, you can do the obvious thing - mix
your solvent layer with dilute acid again and extract back into water. Acid layer could
be evaporated under vacuum to give salts of alkaloids. Alternatively, if the organic
layer were scrupulously dry, bases could be salted out with some organic acid - a
tartrate, oxalate could be formed. I have never bothered with such things - you
would need a lot of pure extract to be bothered. The acid-base extraction process
can be continued as many times as is desired.
If a truly pure product is desired, the only way to go from here is chromatography. I
have never used this at home, and wouldn't think it was worth the trouble, but there
will be papers available on what was used for a particular extraction case.
|Posted by: Nanook Dec 10 02, 01:25 AM GMT|
| San Pedro Alkaloid Extraction For Dummies
v 1.3 - Oct 2002
Note: The title is intended as a bit of tongue-in-cheek humor, and should not be taken to mean that this recipe is easy enough to follow without some basic knowledge of chemistry. You can die.
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.
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, sometimes called "sour salt" and found in the kosher section, 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.
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."
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.