..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:
ii) the JG'92 method: (used on A. maidenii, reported internet 1992)
iii) brief description of the 'E-'93-method': see next post for a more detailed example..
there are also brief descriptions of variations of this method in the Acacia Analysis Thread
in addition:
Phyllode Tek: experiment 1
Phyllode Tek: 'Experiment 2' , taken from Trying to Improve Acacia information p.11:
dromedary wrote:
STB extraction is not suited IMO to Acacia species..although there are some examples around if you search..
nen888 wrote in A. Confusa extraction
..more detail and other methods to come soon..
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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:
"..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)
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 'E-'93-method': see next post for a more detailed example..
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
"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:
..see pic attached below..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.
STB extraction is not suited IMO to Acacia species..although there are some examples around if you search..
nen888 wrote in A. Confusa extraction
nen888 added:Noman (of His tek) wrote at the Lycaeum [http://forums.lycaeum.org/index.phpPHPSESSID=865bbt3igh5i43i2frjbaumpi4&topic=32562.0]:
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..
^..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..
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..and great quote you dug up..
!