yinga (Stranger)
08-09-02 21:23
No 343827
      DMT solubility in methanol and naphtha  Bookmark   

First off sorry for another DMT extraction question but I haven't been able to find this information on here or DMT world or google for that matter.  Anyways I have read some procedures for extracting DMT from mimosa hostilis rootbark and one question relates to the use of methanol to extract the dmt from the plant matter.  Some procedures suggest refluxing this methanol/plant matter mixture.  Would refluxing substantially increase the yields?  Also what is the difference or advantages/disadvantes between using methanol on the ground bark first or dumping the plant matter straight in acidic h20?  Would a warm HCL solution help yields?  Also I have read to warm the naphtha (50C mentioned) before mixing it with the acidic solution.  Would  this also increase the yields or does this just allow more goodies to be absorbed in less naphtha?

(Hive Addict)
08-09-02 23:52
No 343959
      using warm naphta on acidified rootbark wont help ...  Bookmark   

  Using warm naphta on acidified rootbark wont increase yeilds....What it will do is clean it up better so's ya dont end up with alot of fats coming over in your final product.  There will bee the tinyest decrease in your final yield (due to lack of non-DMT fats), but it will bee cleaner product.  Clean is a must!
  The methanol reflux is used so ya have a smaller amount of liquids to work with.  Unless your working on a 1kg+ batch, swim doesnt reccomend this, as it will bee more trouble than its worth.
  If your looking to optimise yields, definatly warm up your naphta when you use it- if its ro###l, make sure its not in the yellow bottle it comes in when you warm it up, or the yellow color will carry over into your final extract.  Whats most important for better yields is taking your time when you extract when it is finally basified, as well as making sure the bark is ground up as fine as you possibly can grind it up.  You can do much quicker extractions by keeping the basified mimosa/naphta warm, but you will sacrifice total yield that way.  Three pulls is enough.  Swim says: first pull, let it soak about 3 days.  Final two, about a week each.
  Definatly do a defat (X3 preferably) and backwash (washing the extract- the naphta that has soaked the goodies from the basified naphta) with slightly basic DH2O in order to get white crystals that slowly turn orange.

ps- MaDMAx says that filtering the hell outta your acidified rootbark will ensure that little or no fat gets carried over.  If you combine the defatting with this, your golden!!

DMT... its good for what ails ya!
Just remember to bring back some of the love.
08-10-02 11:49
No 344087
      The second extractions from the black basic ...  Bookmark   

The second extractions from the black basic solution for me usualy produce the crappy yellow goo when I use NaOH to basify. I usually wait untill the next day to do the second extraction. Would the DMT be more stable if concentrated ammonia is used instead? Also, would boiling down an acetic acid extract of the mimosa cause any DMT to be lost? I was thinking of just boiling the powder mimosa in 5% acetic acid (distilled vinegar), filter, boil down solution to say 1/3 volume, chilling it and filtering it again. Basify, extract with toluene, ect. Does that sound OK? I used to always extract with MeOH first.

08-10-02 11:53
No 344088
      Thanks! I thought the definition of reflux meant ...  Bookmark   

Thanks!  I thought the definition of reflux meant that no liquid would be lost since it condenses again and falls back into the flask?  I also meant to use warm naphtha on the basified solution, not acidic, but you cleared that up as well.  What starting method do you recommend: ground bark into methanol first or skip the methanol and drop it right into acidic h20?
(Hive Addict)
08-10-02 14:54
No 344145
      Holding hands with GOD  Bookmark   

Here ya go, swim wishes he saw something like this when he started out with this extraction. It is written up for someone looking to extract a kg worth of mimosa hostilis rootbark, start to finish.  Scale up or down as needed.

- put rootbark in a canvas bag
- go outside with a hammer
- beat the shit out of bag, making sure the open end is folded under the whole mess, so not too much mimosa dust gets lost
- bust out with a nice, solid blender, preferably one bought at garage sale or salvation army for $5.
- there will still bee longer pieces that havent been pulverised, make sure to fold(break) them over to aprox 1 inch lengths, they will still bee connected by fibers- this is just to help make sure the blades dont get stuck
- tape the lid down to top of blender assembly, if theres a top piece that can bee screwed off, tape that down to.
- unscrew bottom piece of blade assembly
- load ~1/3 or less full with bark- dont pack it!
- screw on blade assembly
- IMPORTANT PART FOR HIGH YIELDS!!!: grind the fuck out of the rootbark
- have a bag handy, no holes in it
- put blender assembly in bag, if its plastic, bee ware! the metal/rubber on the assembly may bee hot enough to melt bag
- unscrew blade assembly in bag, and let contents fall out inside bag, deep inside bag so's the dust doesnt go flying out
- give it a little tap or two to get the loose stuff, dont worry about cleaning the dust that sticks to the sides, do clean that off on your last grind
- reload with bark INSIDE the bag, dont pull the assembly out of the bag, youll get dust everywhere!
- recover and rescrew the blade assembly back on to the pitcher-assembly
- repeat till your out of rootbark

This is swims most efficent method to date for grinding up kg batches of rootbark. Its a pain in the ass, but SO worth it.

Next comes the acidic soak.  He uses a 5 gallon carboy to hold all of his rootbark (1 kg batch).  For smaller batches, one could use 1 or 3 gallon carboys as well, or of course- whatevers convienant.  If one is doing a larger extraction than 1kg grb, then maybee a methanol extraction would bee in order.  Swim has never done this, but one would need a rather large flask,coldfinger unit or sohxlet apparatus.  The rootbark would bee added and refluxed until the MeOH turned a deep red color, and the rootbark started to look leeched (pale-pink/red).  The MeOH would then bee vapped off (reclaim your solvents!) and the resultant goo would bee acidified with enough H3O+ to completly dissolve. 

Swim adds muratic acid to DH2O until pH ~2.  He completly covers the rootbark with it, and then adds about another 1/4 of the total volume.  He lets his first extract sit for about 3 days, then the second and third sit for one week.  Here, heat can bee applied, (gentle heat, use an electric blanket, and wrap the container with it) IF heat is applied, swim reccomends cutting times by three (first extract 1 day, the second and third 2 or 3 days apiece).  When it comes time to change/remove the acidic extract, swim is very lazy.  He uses a siphoning tool that he found at the brewery supply store.  It consists of two plastic tubes, about 3 feet long, one inside the other.  The inner tube serves as a piston, and it is pumped up and down to draw the liquid through the handle and out a plastic hose that is attached to the handle.  Swim only removes the top layer of H3O+ and leaves the rootbark covered.  He collects the H3O+ in a container, and then puts it in the fridge for at least a day, or until hes ready to continue in order to allow the sediment to settle.

When it comes time for him to get the final acidic extract, he siphons as much as possible, then gets a HUGE pot (no Al throughout this extraction, evidently Al can form a salt with acidic solutions and end up in the final extract) and places a CLEAN (washed with no chemicals, soap or fabric softener) army duffelbag with no holes in it, in the bottom of the pot.  (Thanks to DWARFER for this idea)  He places his carboy next to the pot, and has a roll of duct tape nearby.

to bee continued
(Hive Addict)
08-10-02 14:58
No 344149
      Holding hands part II  Bookmark   

Next, he takes the top/opening of the bag and places it over the top/opening of the carboy.  He lifts the carboy beeing careful to keep the bag over the opening, and slowly turns the carboy upside down.  He tapes the bag to the carboy, makes sure its properly propped up, and takes a half hour break whilethe liquid drains.  Think ahead, logistically when you do this!  When he comes back, he removes the tape, picks up the carboy with the bag still in place, and then he takes a long scrapeing tool and empties the grb into the canvas bag.  It can bee quite a chore!  When thats done, he takes a little bit of the extract, pours it back into the carboy and cleans out any remaining scraps with it into the bag.  Next, he takes a thin, strong metal rod, and threads it through 2 opposing eye-holes at the top of the bag.  He twists the bag until there isnt any further slack, and then he uses his bare foot to both pin the bag down while he is squeezing the bag (by twisting the metal bar), and it also serves to help him balance and use his bodyweight to wring out as much extract as possible.  His feet look like hes been making grapes when hes done.  Discard the grb.

Next, its on to filtering, combine extracts and:
- carefully decant into 4 liter sep funnel (or whatever ya got), so as not to disturb sediment on the bottom.
- he has a near 4' stand that he sets up his sep funnel, and 3 filters on. The stand itself can bee placed on a 2 foot STURDY box/shelf so that a carboy or similar type container can bee placed underneath. Both ring stands and regular clamps can serve to hold regular funnels, as well as buchner funnels if you are really careful about it. Double check yourself by wiggling them around once attached.  Swim sets them up in this order: #1 funnel filled with cotton balls, #2 funnel with 2 coffee filters, #3 funnel with 3 coffee filters.
- the sep funnel is situated above the three filters, and when the stopcock is opened, the liquid hits the cotton filter first, the 2 layer filter second, and finally, the 3 layered filter.
- the stopcock is opened, and the liquid is allowed to come out at a moderate speed until swim sees that the third filter is getting soaked. At this time, swim shuts off the sep funnel until he sees how fast the driprate is for the bottom funnel. He then reopens the stopcock so that its driprate is slightly slower than the bottom filter. This is slow, painstaking buisness. You also need to keep an eye on the bottom (slowest) filter every once and a while to make sure the driprate is proper, or youll end up overflowing.
One can also forgo this set-up and vac filter everything X3, but swim prefers this method, as he doesnt like using vac pumps unless absolutly nessisary.

Collect the extract in a large container, and begin your defat.  Two washes is probably all that is nessisary, when swim defats X1, its a crapshoot whether or not he will end up with crystals, or gooey shit (fat).  So do it three times.  Preheat the naphta in a flask, just put it in a warm water bath for 20-30 minutes, luke-warm, maybee a little warmer than that.  First wash, make certain to add the naphta GENTLY.  Ya dont want alot of turbulence when the naphta hits the extract, as an emulsion will likely form.  After the first wash, the danger of forming an emulsion drops considerably, and even more on the third.  Swim doesnt let the defatting process take longer than 24 hours.  He adds the naphta (try using a funnel with a narrow, long spout that so you can try and have the naphta hit the wall of your container, and then drop down onto the extract.  Once again, add about 1/4 of the total volumes worth, when doing a larger extraction, swim will use even less.  No sep funnel needed.  Cover the container, and gently rock it back and forth.  Do that for a few minutes every once and a while.  Let it sit for an hour or so, come back, siphon off (its ok if you accidentally pull off a little extract when your working with big quantities).  If your doing smaller quantities (~400 grams rootbark and less), use a sep funnel.  Repeat 2 more times, but these times, its ok to shake a little more vigarously...a little more!

After the defatting is done, its time to basify.  Swim will take a gallon jug filled about 1/3 of the way with DH2O, and saturate it with NaOH.  He'll let this cool for a bit in the fridge.  Next, add the NaOH solution and watch the pretty colors!  Pour a little, rock/shake a little.  With the bigger carboy, it can bee a pain to get the solution mixed.  You will clearly bee able to tell if its mixed properly or not, because there will be very strong visual indication (color change) where the NaOH is and where it isnt.  Keep going until you see that it has turned a soapy, brown/black/maroonish color.  Its ok if you over basify a little (or alot actually!).  No need for pH papers (if you must, shoot for 9.8-10ish).

to bee continued...
(Hive Addict)
08-10-02 15:27
No 344154
      Holding hands part III  Bookmark   

Once basified, onto extracting the freebase with pre-heated naphta.  Same exact procedure, same exact time-frame as when you acidified the rootbark.  Swim uses ~1/4 of total volume, and does three extractions: 3 days, 1 week, 1 week.  A fourth is DEFINATLY overkill.  Swim experimented on a kg batch, he did a fourth extraction (1 week long) and came up with enough goodies for about 2-3 hits!

Collect extractions, and prepare to backwash.  Swim siphons off the naphta without much care if he accidentally pulls a little of the aqueous solution with it, especially with the last pull.  Any of the basified water that comes over, will bee washed out when you backwash.  Prepare wash water.  Swim uses pH paper for this, he adds IN SMALL AMOUNTS a little bit of NaOH to a gallon jug of DH2O until the paper indicates that its slightly basic.  ~25 grams NaOH (wild guess there) to a whole gallon.  Swim advises use of a sep funnel for this, as the basic water will sink, and it will make life much easier to use the ol' sep funnel.  Three washes.  Swim loads his 4L funnel about 2/3 to 3/4 of the way and nearly tops it off with the basic DH2O.  Swirls it around gently for the first backwash (keeping the tradition), lets it sit about 10-15 minutes, taps off and discards the basic water (bottom layer- once again...).  Reloads, and repeats X2.  More vigarous shaking for the last two.  The color of the Naphta will end up a light yellow when your done with the third wash.

Evap.  Use pyrex baking dishes.  Swim uses 3-4 of them for a kg extraction.  Swim advises one use a SAFE (read:sparkless) fumehood and no heat.  Just leave it at room temp, and let it sit for as long as is nessisary.  If you accidentally pull over alot of fats, it wont crystalise, youll bee left with a wet,waxy mess that is kind of like the consistancy of all natural peanut butter.  Just scrape it up with a razor (itll turn into an orange, wet, goo.  And put it in the fridge.  It will solidify.  Bee warned, that when it once again reaches room temp, that it will revert back to its wet, oily state!
Otherwise, I wont bother telling you what to expect when you do it right.  You will see when your ready.winksmile

DMT... its good for what ails ya!
Just remember to bring back some of the love.
08-10-02 15:42
No 344159
      I'm not sure, I think pure DMT can also be a wax.  Bookmark   

I'm not sure, I think pure DMT can also be a wax. I never waited for it to crystalize. I evaporate the toluene with a fan, I'm left with a thick past but after I repeatily scrap it up and spread it back on the glass it solidifies into a light tan wax. Look at this picture by pkeffect:

Now that's what I call a nice dose.

The DMT in that above photo is most likely pure, but it could probably be molded like a wax. Also notice the slight tanning. Is that a reaction with air? God, does your DMT look more like the above, or below

(Hive Addict)
08-10-02 15:50
No 344162
      Swims crystals often (not always) looks like a ...  Bookmark   

Swims crystals often (not always) looks like a cross between the two.  They will have the crystaline structure/mass as the bottom one, but the crystals will bee clear to off white, and show very slight tints of orange.  Swim is also willing to bet that the stuff on the top picture also had alot of nice-looking crystals in it, just like the bottom pic, prolly centered in toward the middle where the greatest mass crystalized, but ya cant see them 'cause the pic was taken too far away.  A day or so after scrapeing the orange gets a little deeper colored.  Swim would put $ on the fact that rosi@@l was used on the bottom crystals, and the naphta was heated in the yellow plastic bottle.
  The crystals will slowly turn orange as it mixes with air, especially in a warmer environment.

DMT... its good for what ails ya!
Just remember to bring back some of the love.
(Resident Smart Assium)
08-10-02 17:31
No 344193
      >put rootbark in a canvas bag >go outside ...  Bookmark   

>put rootbark in a canvas bag
>go outside with a hammer
>beat the shit out of bag

An alternative method that worked well for me was to take my short lengths of rootbark (a very tough, hard substance) and cut it all up into pea-sized pieces using a pair of tin snips. Regular scissors weren't tough enough for the job, not with the thick pieces I had. Once all the bark was cut up into tiny pieces, I put it into a coffee grinder, about a quarter cup at a time, and ground it into a fine powder. This works great for small amounts of bark, say an ounce or so, and doesn't damage the grinder at all.

I used DCM in my experiment. Didn't do any defatting or anything, just a straight A/B extraction, which yeilded a soft orange wax.

    τΏτ    --  Anger management? Fuck that!
(Hive Bee)
08-10-02 18:34
No 344212
      pure DMT crystals will looks more like this....  Bookmark   

pure DMT crystals will looks more like this....


08-11-02 21:57
No 344546
      not pure?  Bookmark   

wont a straight acid/base extraction leave you with polyponols, terpenes ect as well as alkaloids?
at least thats what my organic chem teacher reckons.

i dont know what to write hear so ill just leave it blank.

(Hive Bee)
08-12-02 01:23
No 344579
      CL's Experience...  Bookmark   

  Well, today, swim ground up 50gms of mhrb and soxlheted it in MeOH till no further color came across (350mls MeOH). Reduce the MeOH down to 200mls and recovered the meoh.

  Next swim acidifies to ph 2.0 w/ 1N HCl.  A series of filtrations w/ filterpaper, cottonball, paper towels ect (4x) leaves me w/ about 100mls of extract.  swim then does a series of warm naptha washes, including 1 w/ naptha75% Trichloroethylene 25% and get a lot of yellow solvent (4x).

  A quick reagent check showes the DMT as a beautiful red/purple color in the acid extract.  swim discovers that swim can accelerate emulsion resolution by laying the sep funnel on it's side an exposing the emulsion to more solvent surface area.

  Swim discovers when it's time to stop defatting by putting 5 ml's in a test tube and hitting with 1 ml concen. ammonia, then adding 5 mls naptha. Shake hard...no emulsion...defat done...

   swim  then basifies w/ 1N naoh to ph 10, and proceeds to extract. does 4 careful extracts.  Reagent test after completion shows NO spice in the Naptha.  The basified mixture shows high levels of spice. Hmmm warm naptha does not seem to be doing much of anything.  A small amount of material precipitates in the naptha (2-3 mgs).  Reagent test shows dmt.

  swim  contemplate this careful process and conclude that the ph is not high enough ( the extract still looks deep burgandy, not gray/black ).  swim then dumps enough NaOH to give a black/gray material.  Begin a new Naptha extraction shake hard...oops now have carmal colored gunk coating inside of sep funnel... big emulsion, letting settle overnight...

Since sep funnel has 3" emulsion,  Swim is prepared as swim bought a centrifuge last week!  Will spin down tomorrow...

  Swim was not interested in week long processes, however some interesting questions came up?

  1.) Why did the spice not migrate to the DCM at ph10?
  2.) Why do the reagents show all the goodies in the basified extract
  3.) Is the black/gray color an essential indicator as to high enough base ph?

  4.) does NH4OH create less emulsion than NaOH?

  more tomorrow..

Infinite Radiant Light - THKRA
(Hive Addict)
08-12-02 05:16
No 344605
      1.) Why did the spice not migrate to the DCM at ...  Bookmark   

1.) Why did the spice not migrate to the DCM at ph10?
  Swiy didnt give it enough time.  Patience!  Even using BOTH warm naphta, and keeping the entire container moderately warm will still take a good week or so to get most of the goodness out.  Did swiy do a thourogh job grinding?  Remember, heat= faster, but less.  If swiy is looking for a quick way for the final extraction, swim doesnt think hes gonna bee able to pull much of anything for at least a full day- especially with such a small amount.  Also, had he taken his time with the initial extraction, there would bee more to work with, plus mechanical losses on filtering (did swiy 'chase' it with H3O+?) with such a small volume on such a small...yadda yadda yadda...
2.) Why do the reagents show all the goodies in the basified extract
  Because thy're still there!tongue
3.) Is the black/gray color an essential indicator as to high enough base ph?
  pKa= 8.68, a little higher than that is ideal.  Swim used to use the pH meter for this, and has found absolutly no significant difference in yield when he has added more base.  Supposivly extra high pH could contribute to formation of emulsion layer- but swim no longer encounters emulsions when doing this extraction -at any point (careful addition of solvents, gentle rocking for 1st and less so for 2nd extraction etc...).  He stopped taking pH when he saw that: the color change occured right around 9-10; and when he went WAY above the pH where this color change occured, his yields and product where the same (backwash is a MUST if swiy does it like that as it washes out all the excess -OH, aint nothing like smoking that shit if it hasnt been cleaned up, DMT burns enough as it is thank you very much).
4.) does NH4OH create less emulsion than NaOH?
  Swims got no clue, never used the stuff for that purpose.  Once again- filter, and bee gentle adding solvents- ESSENTIAL to prevent emulsions.  Swim only recently started beeing anal about filtering -heeding MaDMAx's advice.  Before that, he would just let the acidified extract sit in the fridge, sediment would settle, and hed just decant- even then, STILL had no emulsion problem.  Prevention is the best cure here.  If and when they are formed, swims method(s)(this is for either the defat, the extraction, or the backwash):
- tap off bottom layer into separate container  if that is what is going to bee further worked on- so that it can bee put back into the funnel, or if its during the backwash, just discard bottom (aq) layer.  This is assuming one is working with naphta, the reverse if its DCM.
- tap off emulsion into either a smaller sepfunnel (swim does) or if ya dont have one- another jar or flask
  - add brine to emulsion
  - set it in a warm water bath
  - gentle stirring with a glass rod (swim never does this, but hes heard it recommended several times,so...)
  - filter the emulsion
any one or combination of those last 4 will do the trick, however the most efficient way swim has found is to set it in a warm water bath, and go back to work on the next step, whatever that is.  The emulsion usually clears in an hour or two max if its really thick.  Once again, patience!  Beeing in a hurry can cause one to mess with things so bad (frustration/shakeing/tinkering) that they often get in their own way, it took swim a while (quite a few emulsions)beefore he realised this.
Adding solvent, either brine or non polar is another option if the emulsion is rather small.
  BTW, that tilting thing is also good for speeding up the extraction.  Added surface area....
Also: 50G extraction, highest yield ~460mg, thats if swim didnt take all of them shortcuts.

DMT... its good for what ails ya!
Just remember to bring back some of the love.
08-13-02 03:19
No 345025
      swim also had a hell of a time when he boiled ...  Bookmark   

swim also had a hell of a time when he boiled powdered mhrb in diluted lime juice then tried an a/b with dcm. the emulsions were awful, even after filtering the soln through sintered glass. had similar problems not basifying enough (to pH 11) and failing to extract anything with dcm.
swim left it with a friend and never got the dmt out frown

swim suggests soaking a few days in methanol, vacuum filtering, then following the other bees procedure to defat with naptha, extract, backwash, and evaporate the naptha to get a nice waxy solid. the methanol step is cleaner than acidic water extraction i would think. never dreamt it yet.

adding h2o saturated with NaCl may help break up emulsions. but try waiting awhile and don't shake too hard especially on that the first wash/extraction.
shulgin recrystalizes from boiling Et2O to purify his dmt i think, wink
08-13-02 03:31
No 345031
      Kitchen chemistry (pre-)filter tips  Bookmark   

This is for people who are too lazy to make an aspirator for a vacuum filtration setup & do not have real filter paper but still want their gravity filtration as effective&fast as possible.

A cafetiere is a most useful piece of kitchen extraction equipment. It is made of glass, stands up against prolonged exposure to acidic/alkaline liquids, is stirbar compatible, keeps botanic material submerged during extraction, can be used to squeeze the liquids out of the plant matter (without the risk that acidic/alkaline droplets get on your hands!) and provides in a nice pre-filtering of the liquid.

If you have no lab grade filter paper (Whatman), have to rely on coffee filters then it is a good idea to pour the content of the cafetiere through a empty teabag first, collect the liquid in a container and then pour it through a coffee filter.

This is a much faster approach compared to just coffee filters (which easily get blocked if the liquid is too thick).


(Hive Bee)
08-13-02 10:48
No 345094
      More theory, some ideas...  Bookmark   

  When we look at the problem in any extraction from plant materials, we are faced with lipids, waxes, oils etc.. that are in the material.

   Defatting procedures are suggested to remove the offending lipids.  MadMax's exhortation to filter filter is the use of selective adsorbtion of the higher m.w. substances retained on the cellulose substrate longer than our acidic materials.  In effect, multiple 3d Cellulose TLC plates.

  When I spoke with Dr. S. about emulsions, he replied " You always have emulsions!"  I then asked, "well, what do you do about it?" he pointed to his centrifuge and said, "Use that!".

  Now, what I find is that I have a lot of oil based solvents containing a lot of lipids!  This is not good..wasteful of good solvents, requires additional purification of the solvents etc. waste disposal issues etc.. So there has to be a better way...

  What I have looked into is the use of safeway kitty litter (bentonite clay) as the sorbent medium for retention of the fats and waxes.  Given that the tryptamine has a fw of 188, I plan to use 5HTP in place of the tryptamine, since if I can get resolution with the higher FW compound, then all the better for the spice recovery...

  So, any suggestions as to solvent systems, clay preparation etc. welcome

  Here is the link to a site on clays with info on fat/oil absorption


this line appears in the file: Organoclays consist of bentonite, modified with cationic quaternary amines.

  I have also looked at my Chromo book and it suggests either a cellulose column or an alumina column, giving the solvents for a preliminary clean up...

  Any suggestions on that modification appreciated..

Infinite Radiant Light - THKRA
08-14-02 04:36
No 345318
      Thoughts &Qs on extraction techniques  Bookmark   

The best & most simple precaution against emulsions which pops up in my mind is to use a solvent which is as nonpolar as possible (for A/B). Toluene is a better choice than naphta.

But now I think of it, it would be helpful if some bee can hook me up with some beginners literature on botanical extractions / practical phytochemistry.

In most cases the extractions of crude natural precursors are more difficult to perform than extractions of synthetic mixtures of known ingredients. Botanicals are much more complex and most ingredients are unknown.

Questions which I would like to be able to answer are:

- (when) is it a good idea to first extract a botanical source with the recrystallization solvent of the desired alkaloid, filter out&dry the precipitating powder and then A/B?

- under which conditions is a simple A/B enough and how can that be determined (other than by experiment)?

- under which conditions is it better to use chromatography?

Especially in cases where a lot of botanical material needs to be extracted to get a small amount of mixed alkaloids which then need to be separated I can imagine that the researcher prefers a defatting and/or washing, followed by soxhlet extraction, followed by chromatography and then a recrystallization. This is just an example but many more are possible.

Purifications are the most classic (p)arts of chemistry and all the skills&trics are needed for botanical sources. There are a lot of techniques (A/B, B/A, mixed phase extractions, different forms of chromatography, electrophoresis, steam destillations and specialized oddball techniques such as the Hasenfratz (sp?) method to purify harmine). These techniques can be used in all kinds of sequences.

What I would love to have is a book or database which informs me when to perform which sequence of which techniques for a given botanical start material/endproduct. And if such a database does not exist I would like to know how to select the technique(s) and sequence with potentially the best result.

Is there any literature about that? Preferably as simple as Zubrick?

Please don't tell me to just go to the library and find a bunch of articles about a compound. I know I can do that, but probably I will only find a list of examples of experiments which worked.

What I want to learn is if there is a systematic approach. If I have to test all possible combinations of techniques on each natural precursor / endproduct then it may take decades to find the best one.

Uhhm. Or is this a stupid question and are random experiments the only way to find the grail?    

BTW - what is a good book about the history & development of extraction&purification techniques?

08-14-02 07:21
No 345345
      UTFSE!!!  Bookmark   

Post 308931 (lugh: "Thorpe's", Chemistry Discourse) would bee a good place to start laugh laugh laugh