Hello, hopefully you guys can give me some tips as to how to optimize my next extraction.

First, a quick run through of what I did...

boiled 500 g MHRB powder in ~1 gal pH 4 H20 for about 3 hours while stirring with a magnetic stir bar constantly.

then did 4 pulls with ace brand vmp naptha. for each pull i rotated the bottle and let it sit for about a total of 5 mins.

from there i put everthing in my sep funnel and washed 4 times with pH 4 water. from this I added equal volume of concentrated NaOH solution. the mixture instantly turned milky when the NaOH hit it.

with pre heated vmp naptha i did 4 pulls. The aqueous layer did not really turn to clear though... only slightly, so from there I reduced the volume of naptha in half and stuck it in the freezer.

I got really clean, white crystals. I thought I had way more, but after i let it dry it came up to only .5 g

should I take my time more on the initial pulls?

Your tek sounds similar to the classic Vovins but his method/quantities etc refer to extracting from 50g of MHRB.500g is a pretty large amount to work with.I dunno your extraction history, but IMO, its worthwhile honing your technique by working on smaller amounts initially.

Which acid did you use to get your pH4 water?

You mention an immediate milkiness when the NaOH was added; IME the milkiness changes to a jet-black color if more NaOH is added and its this unmistakable black color which indicates sufficient basification.If your MHRB is not bunk ,and you've not thrown anything away, then nothing is lost.

Have a look at Vovins tek in the Wiki- its a great tek if followed closely at first; later one can be a bit more flexible in ones approach.

I don't think you understood. .. to be more clear i follow lextek because from a (somewhat) chemist's point of view this makes the most sense.

it turns milky after i re-extracted with acidic h20 (citric acid) in my original naptha pulls and add basic water to that. to be expected because I have my DMT in suspension in basic h20 now .. it's going to instantly crash out

I think for the next time ill increase my initial acid bath time by 3 or so hours. I will increase the amount of time for each naptha pull. after the de-fatting step that i am describing, i will probably switch to bestine (heptane) to re-extract because in the past i had much better results using it.

The defat is unnecessary with mhrb, there's essentially no fat to remove.

I'd agree that you should do multiple boils of your bark.

Personally, I'd go with a more straightforward A/B, less fuss, less room for error and just as chemically sound (from a non-chemist's pov on A/B procedures routinely used by chemists )

If you're efficient about your steps there should be minimal lose. I like the de-fat step because i'd have to disagree with you about being low amounts of lipids/fats. In the past, without the step i got a really dirty product

and i'm cursed when it comes to crystallizations ....

I know what you mean though, every time i change phases (basically I do a total of 3 extractions) i'm loosing product ...but thats why i throw in an extra pull each time

Its much more efficient to clean up DMT by recrystallizing with small amounts of solvent then using hundreds of mls of solvent which have to be discarded when defatting. Its an outdated process when it comes to DMT extractions. Even if you had a plant with tons of oil (which is not the case with mimosa rb), you could work the FASA/FASI way and easily separate alkaloids from all the oils and impurities.

Did you do more than one boil, or just one? Did you filter the solids before defatting/adding the base?

Milky solution is a sign of not enough NaOH, you need to add enough so the whole thing is jet black (that seems to be biggest mistake). Add more and pull again.

Also 4 pulls with naphtha might not be enough, do another pull, let it sit for a day with some occasional mixing, and warming it up in water bath.. see if more comes out.

Also a big question is if your mimosa is good in the first place. Is it from a reputable supplier?

I'm just saying...in the non-theoratical, actual result of what you got, there was massive loss, assuming your mhrb is from a reputable source. What should be and what is can be quite different, and when they are, I think it's worth acknowledging.

I'm also saying, there's really not a high lipid content at all. Look at burnt's analysis of jungle spice. Even when pulling with relatively non-selective solvents without a defat, the material is ~95% dmt, with at least ~2-3% being other alkaloids, iirc. This means that even though it may look impure, it's not full of fats/lipids/oils/etc.

Two ideas.

Not enough acid extractions.
Not high enough pH.

Thanks for the replies guys ... I think inadequate cell lysis was the culprit here

Might just be your MHRB mate.

I have done numerous extractions and have tried various things to improve my similiarly crappy yields (I would get just 1g from 500g MHRB....0.2%) but the bottom of it seems to be that my raw material just aint packing the punch.