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LAA isolations, & separations

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V

Vreality

Rising Star
Hello nexus ^_^ !

Thought I'd give a quick intro, missed last weekends reg because I took the weekend off. usually do research and this sorta hobby stuff in the week.

I have a few goals primarily to find the optimal route of purification of dmt.

Ive been looking at things like chromatography and separation via centrifuge.

Still needing to compile the info's here on the nexus that is available that I can find in search out side of my google's but I do know some input from those in the know would also make my search much quicker.

Anyway, i've been looking into which solvents are choice for running dmt through a column. Will be trying out the lime tek shortly here, probably with a pre pressure cook.. Then ill be running clean ups. Then crystallization's once I have a clean up I am happy with..

Goal of clean ups is to have minimal loss of favored alkaloid with optimal color,and smell removal, ( all yellow, red / unwanted gunk that would make end result anything but pure white)

Between active carbon, chromatography, and centrifuge separation there is a route to lab prep grade purification.

anyway just gonna leave that for now great to be among fellow minded fellows cheers nexus.
 
ive done my own little tek write up which is just q21/gordo's lime /white fluff tek with a double freeze and thaw and pressure cook / directions and details for each step.

since ive been getting MHRB work, ive become incredibly interested in HBWR and its alkaloids.

this parrot said dinner would be ready soon so we'll see how things look, ill maybe post my tek its not much new info just some clarifications and made a bit more basic.

biggest thing i think is amazing about the tek is the lack of need of measurement devices really.. you can sorta just eye ball it and itll be fine..


I am very interested in recapitalization and purification's which Ill have some notes on centrifugal purification's and active carbon..

my goal is for colorless tasteless material out side of that I hope to talk to others who work with LSA extractions from HBWR.

I am intersted in doing solid phase extraction of them..
 
now i dont know your background. your intention to use centifuges and chromatography indicates you either know extremely well what you are doing, or maybe, not at all.
just in case i try to give some advise. please try to take no offense if indeed you are knowing what you do and you have access to the needed machinery.


first, i do not know precisely what centrifuge you would need for your purification, but i assume the difference in specific weight between the molecules you want to separate is very very small. in this case, you would need a very powerful centrifuge, and you could (or should i say would) run into deep problems. these machines are not only really really expensive, but also are highly restricted because these are tools you need to enrich uranium.
tbh i think it is dubious you will be able to do it the way you want.

still, doing WHAT you want is quite possible. you wont reach perfect medicinal quality, but you can reach a very high quality.
this is how i do it:
make crude extract. delude vinegar with some water. dissolve your crude freebase in it to transform it to acetate. filter thoroughly. ad some lime or lye to make it a base. no idea what precise ph you need to turn the acetate back to freebase but its not necessary to know it. just add lye by the drop, you want just enough lye to make the freebase crash out*.

at this point, pull with fresh, high quality benzine. do NOT buy cheap diy naphta!. you want benzine that has a certain boiling point range. i prefer benzine with 100°c-150°c. little bit higher would not hurt. anything lower evaporates faster then you can pull, to high, it takes long time to dry. the closer temperature range is together, the higher the quality (if its all the same kind of benzine, it would have a fixed boiling point like water. separation between molecules of similar weight is expensive though. a tight range of 50°c is fine for our purpose)

you wont be able to pull everything, there will be always a loss. i usually do 5 pulls from the purificated solution.


*a magnetic stirrer helps a lot. i got a low quality but very usable stirrer with heating for 30€ on ebay. china ware, delivers worldwide. probably has a shipping center in your country too, shipping will be much faster then (few days instead of few weeks)


ps:
q21 dry tek is 2011 tek, before the discovery of salt. try cyb's salt tek for 33-50% higher yield at the cost of more exhausting pulls.

pss:
eyeballing is bad. a 100g scale precise to 0.1g costs like 7€
for precise dosing, you want a higher quality model. don't trust the numbers they print on them. cheap scales will claim to be 0.01g precise, but they don't deliver.
when i did the research to buy my fine scale it appeared there where no remotely reliable models under 30€, very high precision ones (overkill for dmt dosing) cost 100€

you also want a few pipettes. different sizes are important. you want a large one to get out the bulk. but it will have to high suction, and suck in plant powder. so you need smaller ones too get (almost) all of your benzine.

chemistry baker with scales engraved are VERY helpful. i have 3 (thanks amazon for screwing up the shipping twice and then compensate me by gifting me the first two deliveries) and i do not want to miss anyone of them. i often have different liquids i have to juggle. its nice to be able to make some lye and have it ready when you need some (though, its also dangerous. 100ml are plenty, always have it at a safe and clean spot, and always wear your glasses).

i bought some nice flasks with glass stoppers, because all the teks call for flasks and the lye will eat the plastic seal below the lid of juice bottles. this was a fail purchase. since i have that magnetic stirrer, i do not use bottles anymore at all. the flasks also where more expensive then the stirrer. go figure.
 
i can not tech you the stuff from the start. you seem to have some knowledge. i think, what i wrote will make sense if you try to use the site search to find the teks i mentioned.

many are on the wiki, some on the forum. its hard to judge your knowledge in detail, and i am much more alchemist then chemist when i do my extractions.

the sticky basic extraction background information thread should be your first read, ask once you have made sense of it for further clarification.

the questionnaire also will make sure you at least touch most of the topics you will need. its a great opportunity to verify how much you have forgotten.

i realize i was to motivated to be helpful, and wrote way to much. the right thing to do would have been to suggest to read a few days and then come back to ask.
a few links would have gone a long way. but, i think you should be able to manage now.
 
so my current research is primarily focused on HBWR extractions, optimal Bio reactor techniques, and mutations of Claviceps paspali.



seeing that HBWR is most readily a; im going to go through some different proposed routes..


Ive seen about 3 main routes of extracting HBWR, or other wise isolating it's alkaloids.

Liquid to liquid extraction - Lots of solvent
- Modified by Sohxlet to reduce volume of solvent. ( director of sounds notes) salts out via tartaric

Liquid FAFSA, salting out extraction, using Rotovap to isolate mixed LAA's then FAFSA the desired alkaloids out of the oily impurities. (some mycotopica notes Experimental pure LSA extraction
)


Liquid to Solid Phase - using calcium bentonite clay to grab the desired alkaloids,then Extracting from this clay once dried on fluidized air bed. - Modified; you can use a polymer like XAD4 in a column and extract your desired alkaloid by running your liquid phases through the solid phase collumn. Then you can elute the collumn to get your desired material as it will all be trapped in the XAD 4.

These are my base notes of the general separate possible ways LAA could be isolated to some degree..

may switch thread to myco, so I can write out teks ive found, or refined, and discuss them with out worrying of talking about the wrong things here.
 
alternate source of LAA's production by endophyte fungi isolated form smut grass


Balansia epichloe -

also what maybe responsible for alkaloid production in HBWR seed, as it is a fungal growth in the plant that produces the alkaloid at least as my research has indicated..


It continues to read that Balansia Epichloe has been found to produce major alkaloids while on media that has Tryptophan. Tryptophan has shown in various papers to stimulate major alkaloid production in suspect cultures such as c. Paspali. and Balansia Epichloe.


not the most useful of info, but neat to have available to know it exists.
 
also what maybe responsible for alkaloid production in HBWR seed, as it is a fungal growth in the plant that produces the alkaloid at least as my research has indicated..
Click to expand...

???

Lol, were you living on the moon :lol:

In 2004 the fungi on the vines have been discovered and since then a lot of research has been done on them. They are now named Periglandula as species and belong to the Clavicipitaceae fungi family.

The fungi grow ON the plant, but then get into the seeds for propagation.
 
Aum_Shanti said:
also what maybe responsible for alkaloid production in HBWR seed, as it is a fungal growth in the plant that produces the alkaloid at least as my research has indicated..
Click to expand...

???

Lol, were you living on the moon :lol:

In 2004 the fungi on the vines have been discovered and since then a lot of research has been done on them. They are now named Periglandula as species and belong to the Clavicipitaceae fungi family.

The fungi grow ON the plant, but then get into the seeds for propagation.
Click to expand...
dope. Nice to have snippets of interesting key info in one place. Makes going back to things much easier.

The sarcastic attitude isn't very constructive in this environment.

I additionally noted it, because you read my ref's I put in my post, You can culture it with tryptophan and also get alkaloids just like C.paspali one of those papers say that, but I doubt you bothered to look, just came here to talk down to someone.
 
just came here to talk down to someone.
Click to expand...

lol I always find it funny when people point like that on others, while actually making this themselves. But this is an age old known behavior. Everybody does it. Sri Aurobindo once made a funny comment about this in his aphorisms.

Why do you wanna think so negative about other people?

he sarcastic attitude isn't very constructive in this environment.
Click to expand...

Lol, it also isn't deconstructive, at least not meant like that.

It's just the way I often like to communicate. I can hardly ever be very serious.

And yes, I know, sometimes people don't like it or interpret it as offensive, but that's the way I am. But you can be assured that I don't think negative in any way about anything you said.

Our egos always alter the way you wanna communicate something, that's just how it is. But to get upset about that doesn't make any sense IMHO.

but I doubt you bothered to look
Click to expand...

Again, why so negative?

Sure I had a look at it, but it isn't directly related to the way the Periglandula fungi work (on the mentioned HBWR), that's why I pointed that out.

Don't take things personally, in most cases people don't wanna attack you, but it's ones own interpretation of it. And even if they deliberately wanna attack you, feeling negative about it is the wrong way, IMHO. Just stay happy...is my way on this approach.

As I always say: Egos are like parrots, just a bit more complex. Would you ever get upset about anything a parrot says?
 
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