Acid-Base Extraction of Mescaline from

San Pedro

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."