1014 lines
49 KiB
Plaintext
1014 lines
49 KiB
Plaintext
ftp.u.washington.edu:/public/alt.drugs/chemistry-extracting
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Tue, 02 Mar 93
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TOPICS
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Subject: Alkaliod extraction
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Subject: LSA extraction
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Subject: Extracting alkaloids from Tricocereus cacti.
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Subject: Re: Extracting alkaloids from Tricocereus cacti.
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Subject: Re: Extracting alkaloids from Tricocereus cacti.
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Subject: Extraction Refs
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Subject: Extraction info
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Subject: Extracting DMT from Acacia maidenii
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Subject: Extracting alkaloids from Psilocybe
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Subject: Myristicin and Safrol from Nutmeg / LSA from HBWR
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Subject: Re: Extracting LSA from HBWR
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Subject: Re: LSA
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Subject: BETA-CARBOLINES
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----------------------------------------------------------------------
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From: anonymous
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Subject: Alkaliod extraction
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EXTRACTION:
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The method I use is a general one - I copied it from one
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used by some scientists to extract mescaline from peyote, but I
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have since seen close variations used on many plants.
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This procedure is followed, whenever a plant is studied for its
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alkaloids.
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A few ingredients and bits of equipment are necessary.
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I am a chemist, and have my own chemistry set. I have considered manufacture,
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but I find that there are enough interesting things to do just
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extracting natural compounds, which is much easier, indeed, possible
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in the home.
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You will need:
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A few flasks, glass containers, etc. of suitable sizes, depending on how
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large a volume you are playing with.
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A separating funnel is almost essential - this could be tricky to get without
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a little effort. If you don't know, it is an inverted conical flask with a
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hole at the top to pour stuff in , and a tap at the bottom to let the stuff
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out accurately . It is used for separating immiscible layers.
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A vacuum filtration apparatus would be very useful; I did have a bodgy one
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rigged up myself, but it was always difficult to use. Some kind of still,
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though, is pretty important to have, although conceivably for a once off
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you could get by without it, if you don't mind breathing in a lot of solvent.
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As far as still goes it is to recover solvent, and leave goodness as a
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residue at the bottom. I use a bit of quickfit I nicked: a round bottom
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flask, short column, thermometer on top, and a small condenser... takes
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for ever, but don't expect to follow this procedure in anything under a
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day.
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Other bits and pieces:
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A filtre of some sort is a necessity; preferably a good one, with a vacuum
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pump if you are filtring gluggy stuff (cactus is the worst, sticky goo,
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e.g., other things like seeds and bark are better). People have been
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known to use such devices as coffee filtres, t-shirts, tins with holes
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in the bottom (as a filtre press) and so on. Whatever you can scrounge.
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A lab buchner funnel, sidearm flask, and venturi pump are ideal.
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All this stuff is standard in any chemical lab, regardless of discipline.
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(cont'd in part ii)
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CTION part ii:
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Chemicals necessary:
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The paydirt (obviously)
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Some solvents: methanol (lots), and a non polar solvent. Some people use
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ether - this is dangerous and doesn't dissolve everything. Your best bet
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is probably something chlorinated - I use dichloromethane, although
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chloroform will do (don't breath too much - it is fun at first, but ends
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up making you feel ill). Drycleaning fluid... petrol.... I don't know
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what you have access to.
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Dichloromethane is good because it is non-toxic, volatile, and a good
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solvent. It has a major drawback: separation is often very difficult
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once you have placed your gluggy plant muck in there. The shot is to
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use large quantities of everything, and be patient.
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You will also need an acid (Hydrogen chloride is good)
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and a base/alkali (Sodium hydroxide is good - that way, if you stuff up,
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you end up synthesizing salt instead of something nasty.)
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Also useful: acid/base indicator paper, boiling chips (porcelain grains)
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and activated charcoal - see local chemist.
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The idea is this:
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Most fun compounds (the only exception is maybe THC, and alcohol if you count
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that) are basic - they contain nitrogen.
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So: in general, if you react them with hydrochloric acid, the form a water
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soluble chloride. If you react them with dilute base in the aqueous phase,
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they go back to being a base, which is insoluble in water, but soluble in
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organic non-polar solvents (like CH2Cl2). So, the theory is, that only
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a base will go from water to solvent and back to water etc. when changed
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from acidic to basic and back to acidic. This gives you a way of removing
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all the other crap which is not alkaloid from a sample. That is the theory.
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When I do this, if I can get down to some brown or green sludge that I can
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throw down or smoke, I am happy with a good days work. Ideally, you should
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end up with lovely white crystals, but I think that would require a lot
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of time and effort, and indeed a considerable loss of product in the process.
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Procedure:
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Get your stuff.
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Dry it as much as possible - this makes life easier later on. You will never
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get all the water out, but too bad.
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Chop it up as fine as possible: a blender comes in handy.
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You may wish to chop then dry. A word of caution : try to avoid exposing
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your stuff to excessive heat. I dry in low heat oven. Heat and air destroy
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good compounds from upwards of 100 degs C. All this bit will depend on
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exactly what you are extracting.
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Once it is finely divided - powdered if possible, put it in a big container,
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and cover it with methanol.
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Alternatives to methanol here are ethanol (not as good) and acetone (good
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solvent - rips the crap out of anything, but is more reactive - can react
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with your actives).
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Now, depending on what your stuff is, you have to let the methanol have time
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to remove it all. This is best done by leaving in a quiet warm place for
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a few days, even up to a week, and shaking it occasionally so it is mixed.
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Some papers recommend solvent extraction (soxhlet apparatus) and refluxing
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at the boiling point of the methanol (80 degs or so - I can't remember).
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I usually just rely on time to get the good stuff out.
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When you are ready (early in the morning), filtre the muck, to give you
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methanol+dissolved brown gunk, and a residue soaked with methanol.
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The residue still contains a lot of good stuff, so soak again for an hour,
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and repeat, and do a third time if you are feeling generous (3 is the
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magic number in extraction work).
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When you are done, there is another thing you can do finally, if desired:
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depending on what your stuff is, mix it up with dilute hydrochloric acid,
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1M is appropriate. let stand for an hour, then filtre (this may be very
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difficult) That will get the last of the alkaloids out of the substrate.
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(continued in part iii)
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EXTRACTION part iii
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You now have a methanol-plant stuff mixture, and a dilute HCL-plant stuff
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mixture, if you bothered to do that part.
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Evaporate the methanol, to leave a small amount of goo. This will contain
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water, a bit of methanol, and all kinds of resins and muck, and if you
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are lucky, the alkaloids.
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If a very quick and crude extraction was all that was desired, then after
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stripping the last of the methanol with vacuum if possible, this residue
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could be smoked eaten or whathaveyou. I leave that to your discretion.
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However, if a cleaner product is desired, the double layer extraction
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will need to be performed.
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Combine the evaporated methanol gunge with the hydrochloric acid filtrate
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if you have any. If you don't then mix the methanol stuff with an excess
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of dilute (1M) HCl. Feel free to filtre again at this point. Anything of
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marginal solubility here is no good to you. Get the stuff as clean as
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possible. Boiling with activated charcoal is another useful trick for
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removing gunge. Just boil it up, and filter off the charcoal for a
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cleaner brew.
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You should now have an acid aqueous solution of alkaloids and water
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solubles from the plant.
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Take your acidic solution, and bassify. This is done by mixing in dilute
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sodium hydroxide (I use up to 5M to save on total volume. Be careful with
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conc NaOH - apart from eating skin, it eats alkaloids) As you mix in the
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NaOH, you will see swirls of white precipitate form and redissolve.
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Continue until the white swirls stay, and until the solution is quite
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cloudy. Indicator paper is necessary to see that the solution is basic.
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If you can't get indicator paper, you can make an indicator by boiling
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up some purple flowers. The dyes in most flowers go bright red in acid,
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and green in strong alkali. Just a drop of dye and a drop of mixture
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should tell you what is acid or base.
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The white precipitate is the alkaloids. The more the better.
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Next, add equal volume of non-polar solvent (dichloromethane) to the mix.
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Place in separating funnel, and shake. Separate. This may be very difficult
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or slow. Adding more solvent, more basic water, etc. may help. Adding lots
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of salt to the water layer will help break an emulsion. Ideally you want it
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do this step 3 times - to extract as much as possible from the water layer
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into the organic. I find this part very difficult, and you have to accept
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that you will lose quite a lot of material here. It is, however probably
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easier with some plants that others: cactus is very difficult, barks and
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seeds would be easier. Use plenty of salt, and agitate to separate.
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When you have finished extraction, chuck the basic water layer.
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The solvent layer is kept, and can be backwashed with salty water for a
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cleaner mixture.
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The solvent can now be dried, (using salt or some dry powder, the filtred)
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(I don't usually bother with this - the old hairdryer at the end can
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remove some last solvent and water) then strip the solvent in a vacuum
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to get your final product - some kind of syrup could be expected.
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This is super concentrated, but may only be half the strength of the
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original. e.g. put in enough for 10 doses of morning glory seeds, get
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back 5 doses or more of concentrated alkaloids.
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If it is desired to take the process still further, you can do the obvious
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thing - mix your solvent layer with dilute acid again and extract back into
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water. Acid layer could be evaporated under vacuum to give salts of
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alkaloids. Alternatively, if the organic layer were scrupulously dry,
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bases could be salted out with some organic acid - a tartrate, oxalate
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could be formed. I have never bothered with such things - you would need
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a lot of pure extract to be bothered.
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The acid-base extraction process can be continued as many times as is
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desired.
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If a truly pure product is desired, the only way to go from here is
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chromatography. I have never used this at home, and wouldn't think
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it was worth the trouble, but there will be papers available on what
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was used for a particular extraction case.
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------------------------------
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Date: 08 Aug 1992 17:53:37 -0500 (CDT)
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From: mike@penguin.gatech.edu
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Subject: LSA extraction
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The method is very simple, requires nothing you can't buy easily and legally,
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and it's not very expensive. There are refinements galore to this, and
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I might try them in order to purify this stuff, but the chemicals aren't as
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available, and it rewuires things like pH paper, which I don't know how to get.
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Maybe I can get some anyway. I'll see.
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First of all, you need either (a) a _lot_ of morning glory seeds or (b) some
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hawiian baby woodrose seeds. You also need petroleum ether, which is
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a petroleum refining byproduct, and some high proof drinkable ethanol.
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I'll explain the theory as I understand it so that you can understand the
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flexability in this recipe.
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There are two kinds of solvents, polar and nonpolar. Generally, the good stuff
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in seeds is polar soluable, and the bad stuff is nonpolar soluable.
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So the idea is to first make a nonpolar solution, which of course means
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that you take a nonpolar solvent and soak the ground up seeds in it. The
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result is a solution of garbage from the seeds and the nonpolar solvent.
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Petroleum is a nonpolar solvent, so it will function in this capacity.
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The down side is that petroleum is poisonous, so you don't want to drink it.
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The good news is that petroleum is extremely volatile, so it evaporates
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quickly and cleanly. So the first stage is to soak the ground up seeds
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in petroleum ether for a few days, and then filter the resulting cloudy
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solution through some coffee filters, throw away the solution, and keep
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the seed mush. The seed mush consists of nondisolved LSA's, fiber, and
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the remaining solution that didn't drip through the filter. This part
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can be iterated to get more and more garbage out of the mush.
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The final time, let the seed mush dry thoroughly so that the petroleum
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evaporates so that you don't have any poison in there.
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After the seed mush dries, the nest stage is to make a polar solution,
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which separates the alkaloids (the LSA'a) from the fiber of the seeds.
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This is done with alcohol. There are other polar solvents, but again,
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the key is to have one which easily evaporates, one which will not destroy the
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LSA's, and one which is not poisonous. Ethanol serves this purpose. Methanol
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will also work, but methanol causes blindness, so if you use methanol,
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make damn sure it's all evaporated before consuming the product.
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In some states ethanol is illegal, and California is such a state.
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In that case, using methanol is probably the way to go. Also keep in mind that
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there is such thing as denatured ethanol, which is ethanol which has
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been intentionally poisoned so that it is undrinkable. The reason for doing
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this is that drinkable ethanol is taxable under the Tobacco Alcohol and
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Firearms people, and denatured ethanol has uses in chemistry and cleaning.
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The point is that you should under no circumstances use denatured ethanol
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because it will make you sick or kill you or cause cancer or all three.
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So, make an alcohol solution of the seeds. Then filter the solution
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through filter paper, like before, except this time keep the liquid
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in a jar. Repeat this step 3 or 4 times, always keeping the liquid. When
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you've exhausted the seeds, throw them away. The liquid you have should
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be yellow and smelly. Put this in a shallow flat tray or pan or
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large bowl, and let it evaporate in a dark dry place for a day or two, or
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until there is no liquid. The pan should have a yellowish scum residue.
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That's the LSA gunk. Scrape that up with a razor blade or credit card
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or whatever works. It'll be sticky and gummy, and once it's all scraped up
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it will look dark brown.
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That's pretty much all there is to it. You can take this several steps
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further to get a more pure product. That would be to alternately
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make an acid solution and base salts from the LSA's, which would eventually
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leave you with a very pure white powder. This requires much more effort,
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and wastes some of the product, and the only reason for doing it would be
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to remove more garbage, but the amount of garbage left in the brown gunk
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is insignificant.
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Once you have this stuff as pure as you want it, you can ingest it in
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your favorite form. You can either swallow it as a lump, put it into
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a gelitain capsule, drink the ethanol solution, or dissolve it in some
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cool-aid. I recommend either capsules or swallow the lump if you can
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handle the taste.
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Other notes: Petroleum ether is in Naptha, which is available in
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hardware stores. That's what I've used, and it works fine. Other
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petroleum solvents would work like ethyl ether, which evaporates
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much more easily and is a better solvent, and something like
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gasoline, which has additives and does not evaporate as cleanly as
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naptha. If you can get petroleum ether from a chemical supplier,
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try it instead of naptha. A rule of thumb is that after making a solution
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with the nonpolar solvent, and after it dries, it should smell absolutely
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nothing at all like petroleum, or whatever solvent you used. If you
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use gasoline, you'll notice a strong gasoline smell, which means you're
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screwed. I know first hand from repeated experience that naptha works.
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Also, read the labels of whatever solvent you use. Make sure it contains
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no benzene. Benzene is the most evil carcinogen known, and even in trace
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amounts it can cause cancer. There is no safe amount of benzene.
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On the other hand benzene is everywhere, and if some chemical engineer points
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out to you that there is benzene in naptha even if it's not on the label
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keep in mind that there is an enormous amount of benzene in automobile exhaust.
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You're going to die anyway. If there is no mention of carcinogens or benzene
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on the label of the naptha, then there isn't enough such that you should not
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use it.
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The finer details of this recipe I can give you another time, but I just
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wanted to give you some theory and a general idea of what the procedure is.
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I can give you some things I have from off the net pertaining to this.
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------------------------------
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Date: Tue, 4 Aug 92 12:55:44 EST
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From: JEREMY@RSC3.anu.edu.au
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Subject: Extracting alkaloids from Tricocereus cacti.
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Instructions for purifying alkaloids from Tricocereus cacti.
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This is a general method for concentrating alkaloids, with emphasis
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on mescaline, but which may be adapted to other plants and alkaloids.
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It requires that the alkaloids be relatively basic and that the
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base form be less soluble in water. So it would work well for DMT,
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but not psilocybin of caffeine for example.
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The principle of alkaloid purification is to obtain from a plant only
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that fraction which is basic. This is achieved by a double layer
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extraction, relying on the principle that amines (as opposed to most
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of the other compounds in a plant) are soluble in acidic (the salt form)
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but insoluble in basic (the basic form) aqueous solution. However,
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the basic form is soluble in non-polar organic solvents whereas the
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acidic/salt form is not. Thus, by varying the pH, alkaloids can be
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taken from aqueous solution to organic solution or vice-versa, leaving
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behind other materials.
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Some chemicals and equipment are important for successful extraction of
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alkaloids from cactus. The chemicals include methanol, dichloromethane
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or chloroform, sodium hydroxide and hydrochloric acid. The equipment
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includes a distillation apparatus, a separating funnel, and various
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beakers and containers, pH tester, and filter. Alternatives can
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be found for each of these.
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Method:
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1) Slice and dry the cactus. I haven't worked out the best way to do this;
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no matter how I do it, I am always afraid that I am destroying the
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alkaloids. In general, what seems to work is to slice it thinly, and
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run hot air over it overnight. The more water which can be removed from
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the cactus at this stage, the easier the process will be.
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2) Pulverise the dried cactus. I have tried using a blender, and it seems
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to work moderately well. The cactus is tough so you will have to be
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patient. The finer the grinding, the better the extraction.
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3) Extract dried cactus with methanol. Ideally this is done hot using
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solvent-extraction apparatus (soxhlet). Various makeshift methods
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may suffice for a hot extraction, but I have generally merely soaked
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the stuff for up to a week, cold. Ideally this step should be done
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three times, and the extracts concentrated. I have done it once for
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a week, and then washed out the absorbed methanol with fresh methanol
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once or twice over an hour or two. What you should end up with, after
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filtering out the bulk of the cactus, is a green methanol extract.
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Ethanol or acetone could be substituted for methanol, but neither of
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these is quite as effective. It is generally desirable to use several
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times the weight of the dried cactus for the methanol extraction, or
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at least enough to cover it well in a container.
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4) Remove the methanol to leave just an extract residue. This is best
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done using vacuum distillation, but can be done using atmospheric
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distillation, to recover the solvent. If you don't mind losing several
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litres of methanol, you can merely boil the stuff into the atmosphere;
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just avoid starting a fire. ALWAYS no matter what use boiling chips
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(porcelain) to promote even boiling. Methanol superboils easily, as
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I have found :-(. Once most of the methanol is removed, you will be
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left with a hundred ml or so of watery, methanoly, green slime.
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If it weren't for the methanol and the bad taste, this could be
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consumed at this point. In general, I would say that it may be worth
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your while going to the next stage if you can manage it.
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5) Add dilute hydrochloric acid. Sulfuric acid, etc. could be used instead,
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but I like to use HCl and NaOH, because the product is NaCl, which is
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of no consequence if it contaminates anything. HCl is not as oxidising
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as H2SO4. The HCl should be less than 1M, but not weaker than 0.1M (pH 0-1).
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Add a few times the reduced volume of liquid - e.g. take the stuff
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to 400 ml from 100 ml, etc. One good idea is to let the bulk cactus
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residue (post methanol) dry, and then soak it for a few hours in the
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acid you are going to use to add at this point. This will extract the
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last of the alkaloids. Unfortunately, cactus being what it is, will
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swell enormously, and removing the HCl is tricky. I have resorted
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to large quantities of HCl and a kind of press to squeeze out the
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acid from the bulk residue. This acid should then be filtered, and
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added to the methanol extract residue as above.
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6) (optional) The stuff at this point will be a bit of a mess. Adding
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activated charcoal and boiling gently for 10 minutes will help to congeal
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the chlorophyll etc. which is gumming up the stuff. Do not add too much
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charcoal - less than a gram should be plenty. Too much will adsorb
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alkaloids. Don't use burnt wood, burnt toast, etc - get the proper stuff
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from the local pharmacist. Performing this step will make the next stages
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considerably easier.
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7) Filter the HCl extract. This will remove a proportion of the gunge.
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This will be easier if charcoal was used. The more gunge that can be
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removed at this stage, the better. Washing the residue with fresh HCl
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before discarding, and adding this to the rest will ensure no loss of
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yield.
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8) carefully basify the HCl solution with NaOH. I tend to use around a
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5M solution for this, which is OK as long as you stir as it reacts.
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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.
|
||
|
||
9) 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.
|
||
|
||
10) 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.
|
||
|
||
11) 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.
|
||
|
||
12) 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.
|
||
|
||
------------------------------
|
||
|
||
From: anonymous #2
|
||
Subject: Re: Extracting alkaloids from Tricocereus cacti.
|
||
|
||
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 (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.
|
||
|
||
Hope that's helpful.
|
||
|
||
------------------------------
|
||
|
||
From: anonymous #2
|
||
Subject: Re: Extracting alkaloids from Tricocereus cacti.
|
||
|
||
One other question though which is on "backwashing"... what
|
||
exactly is this procedure?
|
||
|
||
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)
|
||
|
||
Malcolm
|
||
|
||
------------------------------
|
||
|
||
From: anonymous #2
|
||
Subject: Extraction Refs
|
||
|
||
Here are the references for the extraction procedures. I don't have the
|
||
titles of the papers, but all are in readily available journals:
|
||
|
||
Mescaline:
|
||
|
||
JACS 88 p4218 (1966)
|
||
Lloydia 29 p318 (1966)
|
||
|
||
DMT from acacias:
|
||
|
||
Aust. J. Chem 16 p246 (1963)
|
||
|
||
|
||
Malcolm
|
||
|
||
------------------------------
|
||
|
||
Date: Mon, 31 Aug 1992 16:30:46 EDT
|
||
From: anonymous
|
||
Subject: Extraction info
|
||
|
||
>do you know what the following are:
|
||
>
|
||
>Et2O?
|
||
|
||
diethyl ether, commonly called ether. less polar than water or
|
||
alcohol, more polar than petroleum or toluene/benzene.
|
||
I don't use it; dichloromethane is much safer, and easier
|
||
to get, but is slightly more cosoluble with water.
|
||
|
||
>THF?
|
||
|
||
Tetrahydrofuran:
|
||
|
||
O
|
||
/ \
|
||
H2C CH2
|
||
| |
|
||
H2C___CH2
|
||
|
||
It is a cyclic ether, very similar to diethyl ether (obviously)
|
||
but is perhaps a stronger solvent, and is even more dangerous.
|
||
|
||
>IPA?
|
||
|
||
H3C
|
||
\
|
||
H-C-OH
|
||
/
|
||
H3C
|
||
|
||
ispropanol. IPA could stand for anything, but this is a good
|
||
chance. I'd call it iPrOH in writing, myself. It's a common
|
||
alcohol - the next most commonly available after ethanol
|
||
and methanol (not counting sugar etc.). It is still miscible
|
||
with water. Butanol partly cosoluble with water. Higer
|
||
alkanols are not. iPrOH has a similar boiling point to
|
||
ethanol, and is quite volatile. It is less polar than ethanol,
|
||
but much more polar than ether.
|
||
Polarity and solubility is a nebulous concept. If you actually
|
||
look at what is dissolved by what, you can only find vague
|
||
general principles, and plenty of exceptions. Some authors
|
||
have tried to make 3 and 4 dimensional polarity or solubility
|
||
graphs, and put various solvents in various points as having
|
||
a combination of different types of solvent power.
|
||
|
||
>and how to do a distillation "at 2.0 mm/108-112 deg C, or at about 160
|
||
>deg C at the water pump"?
|
||
|
||
You need special apparatus for both. If I were pushed, I could
|
||
put together the latter (I have the necessary equipment
|
||
lying around.) I wouldn't attempt the former, except in
|
||
a lab, which is where I have done it. Both of them are,
|
||
of course, low pressure distillation.
|
||
|
||
At a low enough pressure, anything becomes gaseous. This
|
||
is of course because every substances has a vapour pressure
|
||
at a given temperature. By evaporating something under
|
||
vacuum, you can turn it into a gas at a temperature
|
||
lower than the temperature at which it oxidises or
|
||
spontaneously decomposes.
|
||
|
||
A water pump, or venturi pump, is a simple vacuum which can
|
||
be attached to a fast flowing water source. The
|
||
theoretical minimum pressure is the vapour pressure of
|
||
water at whatever temperature (e.g. 15 mmhg at 20 degs or
|
||
what have you), but in practive, this is never reached.
|
||
A water trap between the pump and the distillation
|
||
apparatus is essential, and if you wish to recover whatever
|
||
you are distilling, you will need a special collecting
|
||
vessel (often ice cooled) as well. A mechanical vacuum
|
||
pump is just the same, except it is large and heavy and
|
||
noisy and expensive and can achive a high vacuum, which
|
||
is often necessary for the distillation and purification
|
||
of organic compounds.
|
||
|
||
------------------------------
|
||
|
||
Date: Mon, 31 Aug 1992 16:31:22 EDT
|
||
From: anonymous
|
||
Subject: Extracting DMT from Acacia maidenii
|
||
|
||
|
||
The following events are as far divorced from reality as the experience
|
||
of the drug itself :-)
|
||
|
||
I discovered that a local plant, Acacia maidenii, was reported to contain
|
||
0.6% alkaloids in the bark, of which 1/3 was N-methyl tryptamine, and
|
||
2/3 was Dimethyl Tryptamine (DMT).
|
||
Alkaloids of The Australian Leguminosae - The Occurrence of
|
||
Methylated Tryptamines in Acacia maidenii F. Muell.
|
||
J.S. Fitzgerald and A.A. Sioumis
|
||
Australian Journal of Chemistry, 1965, 18 433-4
|
||
|
||
Some research of old botany books suggested a nearby location, and to
|
||
my surprise I found many hundred of the trees growing along creek gullys
|
||
in a nearby national park.
|
||
I took about half a kilo of vertical strips from a number of trees, trying
|
||
to cause as little as possible permanent damage. The bark was thick, red,
|
||
fibrous and resinous.
|
||
|
||
Smoking the bark directly gave a mild hallucinogenic effect, on the
|
||
limits of the detectable.
|
||
That evening, I shredded the bark by hand. This was difficult and
|
||
incomplete; mechanical milling would be far preferable.
|
||
I placed the shreds about 3.5 litres of analytical grade methanol from
|
||
Monday night until Friday afternoon. The methanol quickly took up colour
|
||
from the bark and turned a deep red colour.
|
||
As much as possible of the methanol was removed by filtering.
|
||
I evaporated off the methanol using a fractionating column, a condenser,
|
||
and a saucepan of boiling water as heating, for some hours, and recovered
|
||
much of the methanol. I placed this methanol back with the bark and
|
||
reextracted for some hours while evaporating the rest, then filtered
|
||
the bark again and combined the extracts, and stripped as much as
|
||
possible of the methanol, to leave a thick resinous brown liquid.
|
||
A portion of the extract was evaporated using a hair-drier to give a
|
||
thick brown resin. Attempts at smoking this using pipe and hot knife
|
||
proved unpleasant and gave minimal effect.
|
||
|
||
It was decided to perform further extraction.
|
||
To the extract was added dilute hydrochloric acid (about 20 ml 10M,
|
||
but well diluted). Immediately, a large amount of tar congealed and
|
||
was removed, leaving a watery brown aqueous mixture.
|
||
This was basified with NaOH, although on reflection, I would use NH3
|
||
next time as it is less likely to overbasify and react with any of the
|
||
compounds present. White precipitations were seen on basification, which
|
||
redissolved on stirring.
|
||
The aqueous phase was extracted twice into CH2Cl2, and the solvent
|
||
evaporated as before. The last stage of evaporation was accomplished
|
||
with a hair drier, to leave about a gram or so of pale yellow liquid.
|
||
On standing 24 hours, this liquid crystallised as circular arrangements
|
||
of needles.
|
||
|
||
Preliminary attempts at smoking small amounts of the alkaloids gave
|
||
varying mild effects, and a friend and I decided to try a larger dose.
|
||
He took a cone in one toke, and was immediately on the ground, making
|
||
strange sounds and looking odd. He hugged me and told me to meet him in
|
||
that place, and said it was very strong. I managed to finish a large
|
||
cone in 3 tokes, and was instantly blown apart as if by a large
|
||
brick through the head. I think I was temporarily blinded, and
|
||
found myself on the ground grasping my friend, and coughing for air,
|
||
as I watched all of my surroundings fragment into small pieces
|
||
divided by lightning bolts, and feeling all the air in the universe
|
||
escape through the holes. We were both totally astounded and scared
|
||
shitless. 2 minutes later, the intense part was over. We staggered
|
||
out into the open, and walked in the park until we calmed down.
|
||
Pleasant mild hallucinations continued for about half an hour, and
|
||
there were no after effects whatsoever. The experience was extemely
|
||
intense, and the smoke has an unpleasant taste. Several other people
|
||
have tried it since, and the most popular adjective is "wicked".
|
||
Effects have ranged from mild to intense, and some people say that
|
||
while it could not be described as "good" or "enjoyable", they would
|
||
be happy to try it again. My subsequent trips were more bearable,
|
||
as I was not under any anxiety about the duration or outcome of the trip.
|
||
Nevertheless, the trip is still extremely intense, and also physically
|
||
demanding: giving strong tactile hallucinations and stimulation.
|
||
|
||
On a second occasion, I took 1.7 kg of bark, and pulverised it as
|
||
best I could using a circular saw. The result was mostly a fibrous
|
||
powder. Some pieces had to be shredded by hand. Methanol extraction
|
||
was performed as before. Since the amount was larger on this occasion,
|
||
the quantities were somewhat unwieldy. Stripping the five litres of
|
||
solvent (aprx) took approximately 14 hours. On attempting to acidify,
|
||
filter, and basify, considerable difficulty was experienced; the
|
||
acidified residue seemed unfilterable, and when basified with NH3,
|
||
a thick pink gel was formed which was impossible to extract. By a
|
||
painful process of trial and error, I found that at very low pH,
|
||
most of the resins became dissolved or suspended. At slightly low
|
||
pH, the residue separated nicely into a tar and an aqueous phase.
|
||
At slightly high pH, the mixture became a thick gelatinous solid.
|
||
At very high pH, this solid redissolved. The result of this seems to
|
||
be that much of the tar can be separated by successive extraction
|
||
at moderately low pH (dilute HCl), and then that the addition of
|
||
strong hydroxide will leave the amphoteric resins in solution,
|
||
but make the alkaloids insoluble. These are then extracted into
|
||
dichloromethane as before, and the organic layer is back extracted
|
||
with salty NaOH solution to remove impurities. The dichloromethane
|
||
is then stripped as before, to leave the alkaloids which crystallise
|
||
in 24 hours or more.
|
||
|
||
Myself and a friend experimented with repeat doses of DMT at close
|
||
intervals. A base pipe was used for smoking the alkaloids. This pipe
|
||
allows minimum combustion and maximum vaporisation, and thus is the
|
||
most economical way to smoke DMT. Because there is little combustion,
|
||
the smoke does not taste quite as bad, and also the base pipe allows
|
||
more accurate metering of the dose. After the initial physical rush,
|
||
it was found that taking small tokes at intervals of a few minutes
|
||
was sufficient to maintain an extremely pleasant trip, not unlike
|
||
that of psilocin. There was minimum physical discomfort associated
|
||
with the cruise. However, while in this mild state, I took two
|
||
large tokes of the substance, and a few seconds later, without
|
||
warning, I was blown apart. I was walking, but staggered and
|
||
choked, gasping for air. The effects were totally overwhelming,
|
||
like being thrown out of the universe, and I watched my visual
|
||
sphere being pixelated at successively lower resolutions, until
|
||
I could see merely individual elements of colour. The intensity
|
||
was such as to make it very unpleasant.
|
||
|
||
A few more experiences should be related. It seems that the
|
||
response of various people to this extract varies greatly, and
|
||
even a single individual can have a variety of responses, from
|
||
no effect to total dissociation. One girl tried a single toke
|
||
for the first time, and was completely thrown out of the
|
||
universe (from her description). She was begging for it to
|
||
end; the duration was longer than usual: about 15 minutes of
|
||
heavy peak, and at the end of it she vomited while gasping for
|
||
air when beginning to return to some normality and bodliy control.
|
||
|
||
On one occasion, I first ate a whole bottle of the 4:1 extract
|
||
of Passiflora incarnata which is available over the counter in
|
||
Australia. Each tablet contains 500 mg of extract, and I ate
|
||
60 tablets. Supposedly a single tablet is supposed to be a herbal
|
||
sedative, but I was not sedated after consuming the 60. My
|
||
reason for doing this was that Passiflora incarnata is
|
||
supposed to contain a variety of beta-carbolines which are
|
||
mono-amine-oxidase inhibitors, which have been used to
|
||
potentiate the effects of DMT, and make it orally active.
|
||
About 40 minutes later, I smoked some DMT, the effects of
|
||
which were not greatly different from what I am used to.
|
||
I then had a slightly larger amount, and without warning,
|
||
felt an intense incredible rush of physical pleasure through
|
||
my body. Within seconds, I was riding on the most intense
|
||
unimaginable pure total body orgasm. I was unable to control
|
||
myself, and I was screaming at the top of my voice until
|
||
the effects subsided. The visual and auditory enhancement
|
||
were mild, but the physical hallucination is was by far the
|
||
most enjoyable thing I have ever experienced. Observers, who
|
||
were taken aback by my behaviour, claim that I was in this
|
||
state for about 10 minutes. Afterwards, I felt intensely
|
||
euphoric, and both very excited and very relaxed. I tried
|
||
eating a significant quantity of the DMT after this experience,
|
||
and found no effect. This would indicate that the Sedacalm
|
||
passionflower extract is insufficient to orally activate
|
||
DMT at these doses. It may be that higher doses would
|
||
have some effect, or that Sedacalm does not contain
|
||
appreciable quantities of beta-carbolines. Harman,
|
||
harmol, harmalol, harmaline, and harmine have all been
|
||
reported in Passiflora incarnata over the years, but one
|
||
paper claims that only harman, which is not particularly
|
||
active, is the only alkaloid present.
|
||
|
||
I intend to experiment further with this plant.
|
||
I am planning to attempt to side-step the methanol extraction,
|
||
simply by attempting to extract directly into hydrochloric acid.
|
||
Freezing and thawing the bark might serve to burst the vesicles
|
||
containing the alkaloids (if this is the case - I am not a
|
||
biologist). The advantage of doing this would be decreased cost,
|
||
easy availability of all raw materials, and decreased time
|
||
involved. The disadvantage would most likely be a reduction
|
||
in yield, but larger amounts could be processed. The acid
|
||
extract would have to be boiled down from several litres
|
||
to a few hundred mills, then filtered, and this process could
|
||
destroy the alkaloid. Comments on this method would be welcomed.
|
||
|
||
My references tell me that N-methyl tryptamine is most likely inactive
|
||
at these doses. Does anyone have any information regarding the
|
||
physical and psychological effects of this compound? Also any
|
||
information regarding the hazards of DMT use would be appreciated.
|
||
|
||
|
||
------------------------------
|
||
|
||
Date: Mon, 31 Aug 1992 16:35:29 EDT
|
||
From: anonymous
|
||
Subject: Extracting alkaloids from Psilocybe
|
||
|
||
Extraction Instructions for obtaining Psilocin and Psilocybin from
|
||
Psilocybe or Panaeolus.
|
||
|
||
I have not tried this method; it is taken from the classic volume
|
||
(in French) and based on that used by Albert Hofmann.
|
||
Le Genre Panaeolus: Essai taxinomique et physiologique
|
||
par Gyorgy Miklos OLA'H
|
||
Laboratoire De Cryptogamie du Museum National D'histoire Naturelle
|
||
12, rue de Buffon, Paris.
|
||
Memoire hors-series No 10, 1970.
|
||
Page 97.
|
||
|
||
Dry the mushrooms.
|
||
- This important step is most likely to cause the greatest
|
||
loss of yield depending on how it is done.
|
||
Crush or grind the dried carpophores or mycelium to a powder.
|
||
|
||
Shake and allow to stand (e.g. 30 mins) in chloroform. Use maybe
|
||
twice the dry weight in solvents at every step, or enough to
|
||
well cover the powder.
|
||
|
||
Filter and discard the chloroform.
|
||
|
||
SHake the reidue and allow to stand with acetone.
|
||
|
||
Filter and discard the acetone.
|
||
|
||
Shake residue and allow to stand with methanol.
|
||
Filter.
|
||
Shake residue and allow to stand with methanol.
|
||
Filter.
|
||
Shake residue and allow to stand with methanol.
|
||
Filter.
|
||
|
||
Discard residue.
|
||
Combine methanol extracts.
|
||
|
||
Evaporate methanol to dryness, preferably in a vacuum, although
|
||
low heat will do.
|
||
This will yield a crude extract containing the active tryptamines,
|
||
suitable for most purposes.
|
||
This can be further chromatographed on cellulose etc. to give pure
|
||
psilocin and psilocybin. The recommended solvents are
|
||
n-Butanol saturated with water, and n-butanol:acetic acid:water
|
||
(24:10:10). Anyone wishing to do chromatography should check
|
||
the relevant texts for more detailed instructions.
|
||
|
||
|
||
Contact me if you want further information - I may even be able
|
||
to supply it.
|
||
|
||
|
||
------------------------------
|
||
|
||
Date: Tue, 01 Sep 1992 11:20:09 EDT
|
||
From: anonymous
|
||
Subject: Myristicin and Safrol from Nutmeg / LSA from HBWR
|
||
|
||
>can you use an acid-base extraction for getting myristicin from
|
||
>nutmeg or LSA from HBWR? (i.e. are either of those two chemicals both
|
||
>polar soluble and soluble in acidic solution but not basic and
|
||
>whatever the other condition was...)
|
||
|
||
Ok: the former I have tried. The latter I haven't but hope
|
||
to soon. Neither of these is really suitable for the kind
|
||
of alkaloid extraction I have discussed before. In the
|
||
former case, the allyl-benzenes are not alkaloids (as
|
||
you should have realised). In the latter, the compounds
|
||
are water soluble to some extent in the basic form, how
|
||
much so, I don't know. If you look at the method I
|
||
gave for psilocin, you will see it is different from
|
||
that for mescaline and DMT. I got the psilocin recipe
|
||
from an old book. II would have to go back to the original
|
||
literature to make a proper recipe for LSA extraction.
|
||
If you'd like to grab the reference for me (someone at
|
||
Leri is sure to know) then I will go back and check it out;
|
||
the Hoffmann stuff where they first tested obliquhui (sp?).
|
||
TO purify myrsiticin/elemicin/safrole from nutmeg, is
|
||
a tricky process, but not impossible. The shot would
|
||
be to soxhlet extract the oil from a few kilos of
|
||
nutmegs, strip the solvent (pref. under vacuum)
|
||
perhaps filter/press the oil at room temperature
|
||
to remove the nutmeg fats (myristic acid and glycerides)
|
||
Then fractionally distill at reduced pressure to obtain
|
||
the correct fraction. The boiling temperature of these
|
||
components might be a bit over a hundred degrees in
|
||
a strong vacuum. This you could calculate from the
|
||
Clapeyron equation (or a simplified Antione equation)
|
||
and a knowledge of the distillation pressure and the
|
||
boiling points of the compounds at two pressures either
|
||
side of your distillation pressure. I did this using data
|
||
from the Handbook of Physics and Chemistry. The equation
|
||
to use is of the form ln(P/P*) = A/T + B (T in Kelvin).
|
||
This process is quite a tricky one,
|
||
and one which I would not be confident of performing
|
||
succesfully myself. Double distilling would almost
|
||
certainly be necessary to remove the last of the
|
||
impurities.
|
||
If I were to try to purify LSA from HBWR, my first
|
||
instinct would be to grind it, soak or soxhlet (since
|
||
the volume would be small enough to use the reflux
|
||
equipment I have) with methanol, filter, strip the methanol,
|
||
and consume. To go further, without accurate knowledge of
|
||
the substance and its pH/solubility behaviour, would
|
||
be tricky. Chromatography (e.g. TLC) may well be the
|
||
required next step.
|
||
|
||
------------------------------
|
||
|
||
Date: Sun, 06 Sep 1992 21:34:20 EDT
|
||
From: anonymous
|
||
Subject: Re: Extracting LSA from HBWR
|
||
|
||
Concerning the extraction and purification of LSA from HB**,
|
||
The alkaloids are more polar than e.g. DMT or mescaline, and are
|
||
probably water soluble to some extent. Thus, while a crude extraction
|
||
can be performed with methanol, the next stage of purification may
|
||
not be very good. Thus the general extraction method for alkaloids
|
||
is quite possibly not applicable here. That is why I want to have a look
|
||
at exactly what the original method was, although the journal seems
|
||
obscure to say the least. Another day in the Chem Abs section, I
|
||
fear.
|
||
|
||
|
||
------------------------------
|
||
|
||
From: aankrom@nyx.cs.du.edu (Anthony Ankrom)
|
||
Date: Tue, 22 Sep 92 15:41:10 GMT
|
||
Newsgroups: alt.drugs
|
||
Subject: Re: LSA
|
||
|
||
In article <1992Sep22.034310.22075@u.washington.edu> lamontg@carson.u.was
|
||
ington.edu (Lamont Granquist) writes:
|
||
>>[is] there ... a relatively straightforward proceedure to extract the
|
||
>>LSD and get it in a reasonably pure and consumable form?
|
||
>
|
||
>Yup. In a nutshell, you mix the HWBR powder in a nonpolar solvent, keep the
|
||
>resultant gunk(I) and throw away the solution. Then dissolve the gunk(I)
|
||
>into a polar solvent, throw away the new gunk(II) and evaporate the solution.
|
||
>The final gunk (III) that comes out of the solution has LSA in it.
|
||
>
|
||
> gunk(I) = gunk(II) + gunk(III)
|
||
> gunk(III) is the good stuff
|
||
> gunk(II) is not
|
||
> gunk(I+III) are therefore kept
|
||
>
|
||
>nonpolar solvent = petroleum ether
|
||
>polar solvent = alcohol (methanol is better, but is a smidgin poisinous
|
||
> so you've got to be damn sure its all evaporated).
|
||
>
|
||
>I don't have time to give a more detailed explanation than that right
|
||
>now.
|
||
|
||
For the layman: nonpolar solvent also = Zippo lighter fluid.
|
||
|
||
St. Anthony
|
||
|
||
--
|
||
CH3 O CH(CH3)2 | dadaMatrix
|
||
>-P-S-CH2CH2-N< VX |
|
||
CH3CH2O CH(CH3)2 | aankrom@nyx.cs.du.edu
|
||
| A kinder gentler lobotomy...
|
||
------------------------------
|
||
|
||
From: pierre@media.mit.edu (Pierre St. Hilaire)
|
||
Date: Tue, 2 Mar 1993 19:53:02 GMT
|
||
Subject: BETA-CARBOLINES
|
||
|
||
>>Has anyone had a GOOD experience from moderate/large dosages of Syrian
|
||
>>Rue seeds? Was the nausea because of the harmaline, or due to other things in
|
||
>>the seeds?
|
||
>
|
||
>How did you prepare the seeds? Did you boil them and drink the extract?
|
||
|
||
O.K., for all the poor souls who had to ingest those horrible
|
||
seeds, here is an extraction than I think anyone on this newsgroup can
|
||
do in their kitchen without blowing themselves up.
|
||
|
||
From "The Alkaloids" Vol. II by Manske (p393). Printed without
|
||
permission.
|
||
|
||
ISOLATION OF HARMINE AND HARMALINE
|
||
|
||
"The crushed seeds of Peganum Harmala are covered with three times
|
||
their weight of water containing 30 g of acetic acid per liter of
|
||
water [white vinegar is about 50g / l or 5 %]. The seeds swell as they
|
||
absorb the liquid and form a thick dough which is pressed after 2-3
|
||
days. The pressed seeds are once more treated as above with twice
|
||
their weight of dilute acetic acid and, after maceration, the liquid is
|
||
again pressed out. To the combined liquors, sodium chloride [that's
|
||
table salt, man] (100g. / liter of liquid) is added to transform the
|
||
acetates of harmine and harmaline into the hydrochlorides which are
|
||
insoluble in cold sodium chloride solutions and are precipitated
|
||
during cooling. The supernatant liquid is siphoned off, the
|
||
crystalline residue filtered with suction and redissolved in hot
|
||
water. Addition of sodium chloride to the filtered solution causes the
|
||
precipitation of the hydrochlorides as a crystalline mush and this
|
||
process is repeated until the hydrochlorides have acquired a yellow
|
||
color (for the purposes of this newsgroup, once is enough). The final
|
||
product is then recovered by filtration."
|
||
|
||
The paper then goes on to describe the separation of harmine from
|
||
harmaline, but this procedure is slightly more complicated and not
|
||
necessary for most purposes.
|
||
|
||
|
||
Pierre St Hilaire
|
||
MIT Media Lab
|
||
|
||
P.S. While this procedure is legal in the U.S. (where harmine and
|
||
harmaline are currently unscheduled), it is illegal in Canada where
|
||
harmine and harmaline are Schedule I.
|
||
|
||
These are extremely potent alkaloids. Misuse of them can result in
|
||
serious, even fatal, consequences. Read the FAQ about MAO inhibitors.
|
||
|
||
End of ftp.u.washington.edu:/public/alt.drugs/chemistry-extracting
|
||
******************************************************************
|
||
|