I have one old recipe how to extract mescaline from cacti. This recipe is older from first Pedro post here on this forum and also older then Azarius cacti selling repertoire.
In it you can find missing links why and how is mescaline extracted, how mescaline can be extracted in maximum amount.
SORRY CAUSE IT IS LITTLE LONGER
:wink:
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.]
Pulverise 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 oxidising 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.
NOTE:
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 (particulary 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
somesuch.
The final product is a free base. Usually it's unneccessary 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 judgement (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.
*Backwashing- 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)
