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nen888
#1 Posted : 8/16/2012 1:25:18 AM
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..i think it is good to pool all Acacia extraction info into one thread, as they behave differently sometimes to even related plants like Mimosas..

i'm still building this OP, but i will pool all the info from the Acacia Info thread, and various scientific papers into this OP in the future..anyone feel free to contribute/add etc..

methods included will have with certainty 'worked successfully' on a number of ocassions..

i) the 'CSIRO-method' of the late 1960s (as used with Acacias phlebophylla, maidenii etc. ) is briefly described here:
Quote:
"..repeated maceration with methanol. The extract was concentrated, an equal volume of dilute sulphuric acid added, and
after filtration the filtrate was made basic with ammonia. Extraction with chloroform gave
a crude alkaloid solution. The alkaloid was extracted back into dilute sulphuric acid, the acid
fraction basified with ammonia, and extracted with chloroform. The chloroform was evaporated
off to give the alkaloid (40 g(!), 0.3% dry wt.)." [CSIRO 1967]


ii) the JG'92 method: (used on A. maidenii, reported internet 1992)
Quote:
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.

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.

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.


iii) brief description of the 'nen-method': see next post for a more detailed example..

Quote:
1) grind phyllodes/small twigs in a coffee grinder or with mortar and pestle as fine as possible
2) soak overnight in mixture of ethanol/vodka/methylated spirits plus white vinegar and water
3) heat/boil liquid & plant material for approx 45 minutes..keep liquid..add fresh liquid and repeat X 2 (45 min boiling)
4) combine liquids and reduce volume by heating..at various stages here is when as much filtering as possible should be done..e.g. coffee filters (can be slow); reduce volume of liquid as much as possible, i.e until slightly thick..4B) defat x1 with NP solvent - optional
5) very slowly and carefully add casutic soda or pure ammonium until pH between 11-12.5
6) add equal amount of non polar solvent, and separate (optional wash with salty H20+NaOH)..evaporate slow
..all technical issues with emulsions etc are covered in nexus threads..


there are also brief descriptions of variations of this method in the Acacia Analysis Thread


in addition:
Phyllode Tek: experiment 1
Quote:
"A few years ago i observed the following experiment: approx. 180grams phyllodes of 8 year old garden cultivated A. phlebophylla (allowed to naturally dry over a 3 month period) were cut in to small sections with sharp scissors..
they were then covered in 85:10:5 ethanol/H20/acetic acid and allowed to stand for 24 hours..
the liquid was drained & kept and the phyllodes covered in 30:50:20 ethanol/H20/acetic acid and left standing for another 24 hours..they were then simmered at approx 60°C for 30 minutes..the liquid was drained, and the 2nd process repeated.
the 3 liquid fractions were combined and reduced by heat to 500ml of dark liquid..
this was filtered slowly through coffee filter paper several times over a few hours..
the solution was brought to pH 11-12 with the addition of NaOH..and mixed with an equal volume of dichloromethane, and swirled vigorously for 10 minutes..
the dicholomethane was drained and filtered through coffee filter paper..
it was then mixed with an equal volume of basic H20 pH 12 and shaken and allowed to re-separate..the solvent was again drained and allowed to evaporate in a glass petri dish..
this resulted in an unweighed amount of slightly waxy yellow circular crystal formations..these were dissolved in hexane, washed with salty H20 + 1 teaspoon NaOH, drained and cold fan evaporated, resulting in small pale yellow translucent crystals..
vodka may be substituted for ethanol
citric acid may be substituted for acetic
naphtha (the most easily available), d-limonine, or xylene can be used as non-polar solvents.

This information is provided in the interests of research of ethically, sustainably and legally sourced plant material."


Phyllode Tek: 'Experiment 2' , taken from Trying to Improve Acacia information p.11:

dromedary wrote:
Quote:
Building on PrimalWisdom's work I am attempting an A. Cyclops extraction from the leaf material.

250g of fresh leaf material was oven-dried and powderised then left overnight to dehydrate the material of any remaining water. The material was soaked in several washes of excess acetic acid at pH 4. The plant material was filtered out and discarded. The acidic solution was thick and green and smelled like the all the odour a whole tree releases in a week concentrated into a single breath. The solution was basified with NaOH to pH 9 at which point it became black and extremely pungent. Several washes of 100ml NP solvent extracted a strongly yellow transparent solution. Another acid wash left the colouring behind resulting in a cloudy acetic acid solution and a minimal amount of NP solvent on the surface left behind by a hasty decant. Upon rebasifying large amounts of a white solid precipitated and immediately saturated the small remaining amount of NP solvent. The precipitate was dissolved and extracted by repeated washes of the NP solvent.

I am currently waiting for the solvent to evaporate under a cool breeze.

Quick update: I had a bit of a solvent problem - tried a new brand which apparently does not dissolve very much DMT at all. I should have noticed that the cloudiness of the basic solution was not visibly reduced by repeated solvent pulls, oh well. That evaporation yielded less than 50mg of product, most of which was wasted trying to get it out.

Now with a better solvent and access to a freezer I've repeated the entire process and finished with freeze precipitation. I have noticed after 24 hours a bunch of pure white beads the size of pinheads at the bottom and dense cloudiness that suggests there is more to come. As part of my attempt to force more DMT to dissolve in the bad solvent I salted the basic solution with NaCl until it was dense enough that all the DMT precipitate has risen to the surface of the basic solution, still sitting tantalisingly under the solvent. I wonder if I can scoop it out somehow.

[nen888 adds]: ..keep up the good work dromedary..it may be better to separate the solvent layer with the precipitate (plus a little bit of basic solution), and then mix with slightly basic water and re-separate..some shellite brands do not seem to be a particularly good version of napatha for alkaloid holding capacity, lighter fluids are usually better..

[dromedary continues]: I've retrieved 250mg or so of white powder from the A. Cyclops so far. It smells like DMT but I won't be doing an assay until after Christmas.
..see pic attached below..


STB extraction is not suited IMO to Acacia species..although there are some examples around if you search..
nen888 wrote in A. Confusa extraction
Quote:
Noman (of His tek) wrote at the Lycaeum [http://forums.lycaeum.org/index.phpPHPSESSID=865bbt3igh5i43i2frjbaumpi4&topic=32562.0]:
Quote:
It's not much of a coincidence that nobody started talking about DMT N oxide until STB teks started to become popular.
Yellow oily extracts are common with STB's - especially from solutions that have sat for awhile and/or are extracted warm. The intense alkalinity of the solution breaks he bark down so far that plant material that would otherwise be insoluble in naptha is extracted. Heat has the same effect.
These plant materials carry with them some of the alkaloids - whatever they may be - that constitute jungle or dark DMT, which is usually only extractable using a wide spectrum solvent like xylene.
When alks of dark DMT and NN DMT are combined, they form a yellow/orange goo that will never solidify. Separate them with heptane and you get crystaline NN and sticky powdery dark.
I'm not saying that none of the yellow found out there is oxide, but I'm willing to bet that the majority of it is simply NN with residual plant matter in it and a smattering of jungle alks.although there are a few reports of STB if you search..
nen888 added:
Quote:
^..but in the case of A/B Acacia extractions, the most likely non-solidifying factor is NMT..a perfectly groovy alkaloid..just not as 'strong' as DMT..just be patient crystalising, and xplore the difference..


..more detail and other methods to come soon..

.

.

nen888 attached the following image(s):
sp. aff A. cyclops extract 2011.jpg (456kb) downloaded 4,615 time(s).
 

Trippy glass for trippy people.
 
nen888
#2 Posted : 8/17/2012 2:54:45 AM
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the Phyllode Tek Experiment 3

plant material..a friend and i observed an interesting looking small population of Acacia maidenii in NSW..this population shares some characteristics with A. obtusifolia in that it's pods are less coiled than typical maidenii (though not as 'straight' as obtusifolia, which typically has mildly convex pods), but it's phyllodes are not as thick and leathery as obtusifolia, nor blunt (as in the meaning of obtusifolia)..
it has been previously seen flowering in spring (September)

recently, i witnessed an experiment in which the leaf and twig were extracted as follows:

..500grams of A. maidenii phyllode and small twig were crumbled and broken by hand..leaves would have averaged 3-5 'breaks'/sections, meaning it was not especially finely ground/processed
..the material was covered with ethanol/H20/vinegar 90:5:5, and allowed to stand for 2-3 hours..
..the solution and plant material were then heated at approximately 70-80 degrees C, allowing the ethanol to boil..it took a medium red colour, around 2.3 litres..
..the liquid was poured off, reduced in volume by 75%, and filtered several times through unbleached cotton..a large of amount of particulate matter/tar amd gum was collected in the filter and discared..the volume was reduced to 300ml and brought to ph 5-6 with vinegar (a small dash)..this was labled ∂ (alpha)
..the plant material was then shaken with 250ml of ethanol for 30-45 seconds, this was discarded and combined with the first lot of liquid..
the phyllodes were then covered with H20 and approx. 100ml vinegar, and allowed to stand for 16 hours..it was then boiled for 40minutes..it took a golden/red colour with a slight milky cloudiness..
..the liquid was again poured off, reduced, and filtered several times..far less tar/gum was caught than in the alpha extraction..it was reduced to 300ml, final pH 5..this was labled the ß (beta) extraction..
..both acid solutions were then brought to pH 12-12.5 with NaOH/H20 solution, allowed to cool to room temperature, mixed with equal portions of dichloromethane, violently shaken for 10 minutes, and left to stand..clear separation of polar/non-polar layers took approx 1-2 hours..the NP solvent took on a mild yellow colour in both..
..the NP solvent was drained, washed once with H20/NaOH/NaCl solution (pH 8 ), re-separated after 20 minutes, and evaporated with a non-heat fan..
..after around 12 hours both extractions were a yellowish oil, though ∂ had more yellow, and signs of gum still congealing (pale brown paste)
..so..the results..?
∂ resulted in 30-40mg of a yellow/beige 'toffee' which would not completely solidify after another 24 hours of standing..experience and bioassay suggested that it was probably at least half nmt (n-methyltryptamine)
ß resulted in almost 1.5 grams (yes, 1500mg) of mainly off-white dmt soft crystals, with small amounts of yellow conglomerations..crystalization was sped up by scratching the surface of the 'oil' with a needle..later assay suggested mainly dmt, though it did not completely solidify, reverting to 'putty', often caused by nmt with betacarbolines, and perhaps trace fatty acids..these do not detract from the experiential aspect..

..a third 'pull', with 40minutes heat as in the beta, resulted in maybe 50mg alkaloid at most, so esstentially the ß extracted most of the alkaloids..

the percentage, then, of this A. maidenii was around 0.3% [from phyllode/small twig 80:20]..qualitively it was probably, in the case of the ß at least 85% dmt,with probably some nmt (slight duration extension and extra spatialness) and trace betacarbolines (as suggested by a slightly slowed onset at assay, and again slight time extension..according to the bio-assayer)

so, this would suggest, amongst other things, that some tests would find only a small percentage, not going through the extra stage as described here..also, it suggests that water slightly fortified with ethanol and a dash of white vinegar is the preferred solution..

..some brands of methylated spirits (95% ethanol) can be substituted, check carefully for residues;
methanol is the most efficient but is very poisonous and has no smell, so should not be used outside of safe lab conditionsl..due to reaction problems caused by some acids with acacias specifically i would suggest using (for now) only either acetic, dilute sulphuric, or citric acids
..as far as non-polar solvent choices go, hexane and xylene will work as well as described above in place of dcm; naphtha will usually require 2-3 pulls or extractions from the basic solution, whereas these other solvents require often only 1 solvent washing (they have a higher 'holding capacity', or solubility ratio)
..d-limonine..endlessness has achieved very good general dmt extraction results with the more 'natural' d-limonine (NP solvent derived from oil of lemon/citrus, naturally occuring in traces in the rind) ..this is perhaps what 'from plant' purists & organicists best use..
..chloroform is the common scientific standard NP solvent for such tasks, but should not be exposed to sunlight or left standing for long with alkaloids, or can react, as can to a lesser extent other chlorinated hydrocarbons..
for more detail on basifying alternatives to NaOH (some potentially less harsh)
and solvent choices/comparison, search the extraction subforums of the Nexus..

..hope this info is helpful, encourages sustainable leaf teks, and leads to less likely wastage of long grown plant material through inefficient or failed extraction..

please be kind to trees and grow them..



 
r2pi
#3 Posted : 8/17/2012 11:46:39 PM
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How bad would it be to use water instead of ethanol? Could finer chopping (e.g. stick mixer once wet) help make up for the poorer solvent? I have to do my boils with a gas stove (outdoors) so I'm guessing 90% ethanol would be a no-no!
 
endlessness
#4 Posted : 8/18/2012 1:34:26 AM

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I bet any standard A/B tek would work decently for acacia but I never tried it to know for sure. I would make sure to break well enough the material, 3x boil or pressure cooker, pull with appropriate solvent. If you just want DMT, naphtha etc should work fine, or something like limonene/xylene and then salting out (FASA/FASI would be good if plant was very fatty/oily). You can always recrystallize if necessary. If you want more full spectrum (acacias often have other alkaloids like different tryptamines and b-carbolines) then you must use a solvent at least like limo or xylene, or something like DCM.

Did you or others ever try standard a/b nen?

Anyways its def important as nen said to harvest sustainably too.
 
nen888
#5 Posted : 8/20/2012 12:49:45 PM
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..r2pi wrote:
Quote:
How bad would it be to use water instead of ethanol? Could finer chopping (e.g. stick mixer once wet) help make up for the poorer solvent? I have to do my boils with a gas stove (outdoors) so I'm guessing 90% ethanol would be a no-no!

..you can use just water with a little white vinegar (to make the alkaloids more soluble in salt form), but this may require more boiling to get alks out (see my comment on heat below)
..ethanol requires less heat/time and no acid (there are reasons one may not want to acidify)
also, 90% ethanol with H20 will not easily catch alight (like 100% ethanol)

endlessness
wrote:
Quote:
Did you or others ever try standard a/b nen?
..i have, and it usually 'works', but in my deep search for the 'purest' expression of what was actually in the tree i've noticed a few things which may be specifically an Acacia-thing, or rather certain species..Acacias maidenii, otusifolia, mucronata and longifolia in particular appear to change with excessive use of prolonged heat, and acidity (especially the combination)..there seem to be changes to some of the other alkaloids present which i don't find desirable (though these aren't extreme)..generation of extra betacarbolines and odd complexes between condensed tannins and tars can be created..i'm still planning to have all this tested one day..but, this changes seasonally..it's hard to pin down, hence so is a same-every-time tek..
so, as a kind of 'purist' i now find better results from as less heat..but if it was P. viridis in the pot i'd boil the hell out of it..generally, though, i'm an extraction 'rock-n-roller' rather than a formula/numbers type..i like to Experiment..
i really hope people with successful results and different methods will post their results also..

..here's a link to DoingKermit's Confusa Extraction, which is a fairly standard A/B and seemed to work well..
 
Seldom
#6 Posted : 8/20/2012 1:30:02 PM

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the more i look in to it i think the herbalists are ones to look to, a good understanding of solubility for the different elements of a plant's composition is a good place to start, for eg. see nen's post in the acacia thread about alkaloids and plant tars/resins
http://www.innerpath.com...Herbalmanufacturing.htm

Quote:
SOLUBILITY OF PLANT CONSTITUENTS

Glycosides: Most are soluble in water and alcohol. Glycosides are rendered inactive, or become less therapeutically active, by hydrolysis in water and must therefore have a sufficient quantity of alcohol for preservation.
Saponins: Saponins froth when shaken in liquid. They are neutral and soluble in water. Saponins undergo hydrolysis in water forming sugar and precipitate.
Enzymes: Soluble in water and insoluble in alcohol. Enzymes are usually destroyed by temperatures of 70°C or greater.
Alkaloids: Soluble in alcohol and slightly soluble in water. Alkaloids are generally in the form of alkaloidal salts in plant material which are soluble in alcohol and water. Alkaloids extract well with a water/glycerin solvent. They may be unstable when heated.
Anthraquinone derivatives: Soluble in water and alcohol. Not all anthraquinones are stable when heated and may be stable in an infusion, but not a decoction.
Tannins: Soluble in water and glycerin. 5-10% inclusion of glycerin to a menstruum increases the action of tannins and prevents precipitation after prolonged period. Some tannins are insoluble in alcohol and may break down with prolonged heat.
Volatile oils: Soluble in alcohol and glycerin and only slightly soluble in water. Volatile oils vaporise with heat.
Resins: Soluble in higher strength alcohol and insoluble in water. Resins melt near boiling point.
Gums: Soluble in water. In their liquid state in plants are MUCILAGE. In their dry state GUM. Gums are insoluble in alcohol and most organic solvents and coagulate with heat.
Proteins: Soluble in water, insoluble in alcohol and are coagulated by heat. Proteins are not used in preparations as they are inert, undergo putrefaction, may aid decomposition and increase bulk.
Fixed oils: Fixed oils are mainly found in seeds and fruits. They should be defatted before extraction with alcohol. Fixed oils are insoluble in water and do not vaporise with boiling.


an interesting one: http://www.erowid.org/ex...iences/exp.php?ID=52303

FASA or FASI https://www.dmt-nexus.me....aspx?g=posts&t=2546
 
nen888
#7 Posted : 8/20/2012 1:40:31 PM
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..hey, you're a smart cookie SeldomSmile..and great quote you dug up..
another thing suggested by the 'Phyllode Tek' Experiment (& your quote) is that the tars/gums have are much easier to remove from an alcohol solution..the conditions of the experiment lead to the alpha step removing most of these, allowing the beta step to cleanly extract the alkaloids..
 
acacian
#8 Posted : 9/4/2012 7:54:04 AM

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hey nen.. regarding the original dmt findings in maidenii, I have read from various sources that the original maidenii trees found with dmt were later revisited and found to actually be obtusifolia? Do you know if this was actually the case? or do you think it may have been one of the active strains of maidenii/maidenii x obtusifolia, and that maybe obtusifolia grows in the same area and this was more of an assumption based on its presence in the general area
 
acacian
#9 Posted : 9/6/2012 9:44:55 AM

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Seldom wrote:
the more i look in to it i think the herbalists are ones to look to, a good understanding of solubility for the different elements of a plant's composition is a good place to start, for eg. see nen's post in the acacia thread about alkaloids and plant tars/resins
http://www.innerpath.com...Herbalmanufacturing.htm

Quote:
SOLUBILITY OF PLANT CONSTITUENTS

Glycosides: Most are soluble in water and alcohol. Glycosides are rendered inactive, or become less therapeutically active, by hydrolysis in water and must therefore have a sufficient quantity of alcohol for preservation.
Saponins: Saponins froth when shaken in liquid. They are neutral and soluble in water. Saponins undergo hydrolysis in water forming sugar and precipitate.
Enzymes: Soluble in water and insoluble in alcohol. Enzymes are usually destroyed by temperatures of 70°C or greater.
Alkaloids: Soluble in alcohol and slightly soluble in water. Alkaloids are generally in the form of alkaloidal salts in plant material which are soluble in alcohol and water. Alkaloids extract well with a water/glycerin solvent. They may be unstable when heated.
Anthraquinone derivatives: Soluble in water and alcohol. Not all anthraquinones are stable when heated and may be stable in an infusion, but not a decoction.
Tannins: Soluble in water and glycerin. 5-10% inclusion of glycerin to a menstruum increases the action of tannins and prevents precipitation after prolonged period. Some tannins are insoluble in alcohol and may break down with prolonged heat.
Volatile oils: Soluble in alcohol and glycerin and only slightly soluble in water. Volatile oils vaporise with heat.
Resins: Soluble in higher strength alcohol and insoluble in water. Resins melt near boiling point.
Gums: Soluble in water. In their liquid state in plants are MUCILAGE. In their dry state GUM. Gums are insoluble in alcohol and most organic solvents and coagulate with heat.
Proteins: Soluble in water, insoluble in alcohol and are coagulated by heat. Proteins are not used in preparations as they are inert, undergo putrefaction, may aid decomposition and increase bulk.
Fixed oils: Fixed oils are mainly found in seeds and fruits. They should be defatted before extraction with alcohol. Fixed oils are insoluble in water and do not vaporise with boiling.



which of these are undesirable in extracts? this is really interesting info to know for ridding extracts of unwanted chemicals
 
nen888
#10 Posted : 11/1/2012 11:07:16 PM
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^..you certainly don't want Resins, really don't want Gums, and best avoid Tannins (as they keep pushing down the PH)
..there's also Waxes, which can get in the way, but, in acacias, don't seem otherwise harmful..
 
nen888
#11 Posted : 11/1/2012 11:07:57 PM
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the Phyllode Tek.. Part II

experiment 4

material: A. floribunda narrow phyllode dry (3-4 months old) approx. 250grams.

method: leaves ground in coffee grinder, in portions; soaked overnight in a mixture of 50% non-cloudy vodka, 40% rain water, 10% white vingegar; boiled vigorously for 45 minutes, re-covered after draining in same ratio, boiled vigourously for 70 minutes; liquids combined and reduced to half volume by boiling; filtered twice through coffee filter paper (slow); reduced in volume until slightly thick; cooled, NaOH added very slowly until just above pH13; cooled, an equal portion of dichloromethane added and the mixture shaken violently for 10-15 minutes; allowed to stand and separate; dcm (now pale yellow) drained and washed with salty water+NaOH; dcm drained and fan evaporated to yield a few hundred milligrams of brown waxy crude alkaloids; these were re-crystalised from dichloromethane to yield a dark semi-crystalline material which took 5-6 days to completely solidify.

bioassay: 50-60mg of the material were vaporised by a test subject in 3 inhalations resulting in pleasant tryptamine-like effects and tapestry visuals; onset over around a minute and afterfeeling to 60 minutes (as well as colour of extract) suggest some betacarbolines present.

afternote: the plant was not in flower when leaves were collected.
.
 
acacian
#12 Posted : 11/2/2012 6:55:44 AM

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been investigating nen's idea of extracting a purer expression of the plant. this idea of being non-discriminate of the plant's wisdom-on-offer really resonated with me and my beliefs about plant consciousness, chemical profiles and the intention behind these particular alkaloid profiles.. so I thought I would have a go myself with an alpine mountain dwelling species of acacia which I know is fairly consistent in its alkaloid yields.

82grams of dried acacia bark was ground to a near powder. The bark was poured through a funnel into a large glass bottle. 700ml of methylated spirits, 100ml water and a dash of vinegar were added, and the bottle was shaken in a "swirl" fashion periodically over the next 6 hrs before being poured off and transferred to another vessel. 500ml ml of fresh methylated spirits were then added as well as a dash of vinegar. ph 4.5. The process of shaking and sitting was applied for another 5 hrs until being poured off and replaced with another 500ml. All up 1.65 litres of methylated spirits was applied for the soaks. The solution ended up clear yellow after filtration. It was then reduced on low heat to 340ml and re filtered again through coffee filters. It ended up a dark red colour. The ethanol solution was then diluted with 150ml water. final ph 4 (keep aiming for 5 but always adding a little too much... literally a small dash of white vinegar brings the solution to around ph 4)

The solution was then defatted first with 100ml xylene then 60ml. The xylene went a bright yellow colour and was removed upon separation of layers. 11g caustic soda was then added to the defatted acacia solution. A large amount of precipitates formed creamy clouds in the solution before dissolving and then turning black. The final ph came out at 12.9. The solution was left to sit for 15 minutes.

100ml xylene was then added to the basified solution. mixed throughly and allowed to separate twice, before the xylene was pulled from the solution. this process was repeated with two lots of 100ml xylene. The xylene was then placed in a square pyrex dish and slowly evaporated


... will probably take a couple days as xylene is a bit of a snail when its comes to evaporating. will post results when its done


next experiment will be from the phyllodes of a gorgeous acacia floribunda from the warrendyte area in victoria. I've been unfortunate to not get anything yet from the floribunda so far.. though it seems there are a lot of differen't genetic variants. this particular one has a "teacher" vibe to it and has very white creamy flowers, so I'm hoping it can yield something worthy of teaching Smile its not in flower in anymore either

oh.. and kudos Nen for using rainwater! I used the water that flowed from the waterfalls of mt buffalo for my last extraction. I haven't tried the extract yet, though I took every measure (other than solvent choice.. i only had shellite and had no money for other solvent) to ensure optimal "purity".. spent a long time on the brew and worked harder at pouring my intentions into the extract. I ended up with easily the nicest fluffy snowballs I've gotten so far!
 
nen888
#13 Posted : 11/2/2012 9:27:13 AM
member for the trees

Acacia expert | Skills: Acacia, Botany, Tryptamines, CounsellingExtraordinary knowledge | Skills: Acacia, Botany, Tryptamines, CounsellingSenior Member | Skills: Acacia, Botany, Tryptamines, Counselling

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..actually, it may not have been my experiment Wut?

thanks for that report acacian..i stand by for more..
.
 
acacian
#14 Posted : 11/8/2012 9:19:28 AM

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xylene STILL evapping ... lastnight i accidentally left the dish out in the garden and it rained... some drops went through the cloth into the solvent. so i decanted it from the dish leaving the water drops. upon touching with my finger the droplets left white smudge marks in the dish.. so it seemed that they had pulled a small amount of the alkaloids. must have been slightly acidic. i poured vinegar into the dish and swirled round thoroughly for 20 minutes and then basified the vinegar and reextracted with more xylene.. i added that to the other xylene that i decanted. evapping again. the spice that the rain drops pulled was definitely minimal .. .. but i'm glad i recovered it. i did a second pull but its yet to be separated. I'm prettys sure i've got all of it as the first pull would have pretty much gotten everything.

currently performing an A/B on Acacia Alpina will post results soon
 
phyllode
#15 Posted : 11/8/2012 11:36:39 AM

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^ What about fan evap. solvent Acacian?
Not bush doctor enough for this journey Smile?
The suspense is killing us! ha ha
 
acacian
#16 Posted : 11/8/2012 9:58:11 PM

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il chuck a fan over it today and leave it in the sun. its basically taken a whole week now. I am really looking forward to it finishing. the fan never seems to make a difference for me with xylene though
 
acacian
#17 Posted : 11/9/2012 3:15:16 AM

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well. i am angry with myself thats all i can say. beautiful day today... very sunny and warm.looks like todays the day for the xylene to finish...its been a longtime in the waiting, but we're on the home run now. left the dish out this morning to keep evapping with the cloth over the top... and whaddya know a couple hrs later it has almost finished evapping and it rains again while I am inside... i realise pretty qucikly and tend to it and do a quick pull from the water thats leaked in again (once again a minimal amount) and get the xylene re-evapping, this time under a fan. i go into the kitchen afterwards, where my alpina brew was reducing.. and it had burnt to a crisp. not happy jan.. really... not...happy. what a waste of a beautiful plant. sorry alpina..

also spilt a very small amount of the xylene .. i wiped it with a piece of toilet paper and squeezed into teh dish. whatever was lost was minimal. but boy.. that alpina extract, i was really looking forward to finding out whats in it. and i had not planned on going back to mt buffalo until after december. early afternoon beer for me
 
zombicyckel
#18 Posted : 11/9/2012 3:26:59 AM

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acacian wrote:
early afternoon beer for me


Sounds good Very happy!
 
acacian
#19 Posted : 11/9/2012 4:31:24 AM

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stupid melbourne and its patchy weather. it happened again in the tiniest time frame it was sunny as one minute pouring the next.. the conveniently cleared up again after drenching the extract. over this. i hate xylene. i hope theres goodness left in it...
 
Major Tom
#20 Posted : 11/11/2012 6:27:55 AM
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I read above somewhere of some body having difficulty powdering bark . If one has a bench grinder or an angle grinder , wire-brush attachments are available that do the job beautifully . Just grind the dust into a bin or box for ease of collection ; and be sure to wear a mask and eye protection...Thumbs up
 
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