About to make my first A/B (mesembrine), help would be very appreciated!

[Kneegrow]

Hello, SWIM is about to make his first acid/base extraction. He has been reading here in the forum for a while now and made his own little tek, some verification would be wicked!


1. ACIDIFICATION: Acidify destilled water with acetic acid (He does this until the pH turns to approx. pH 4? And for this step he'll be using sulphuric acid when he has built enough experience). He then adds the acified water to the plant parts. Let it stand for an hour or two (maybe more, can someone confirm?). Filter everything through a t-shirt and then a coffe filter. Repeat this step 2 more times to get everything out from the plant parts and then combine the acified liquids.

2. DEFAT:
Add approx. as much naphta as the acified liquid (can someone please confirm the amount?) This will be mixed together and then put into a separatory funnel and shaken (does he have to do this very gently to make sure he gets no emulasion or it doesn't matter?) Ventilate now and then to release pressure. Put in hot water bath. Discard the naphta and keep the acidified solution. Repeat 2 more times or until the naphta isn't yellowish any more.

3. BASIFY:
In the acidifed solution he then adds some sodium carbonate diluted with a tiny bit of destilled water until the pH of the whole mixture reaches 11 (would sodium carbonate work fine or should I find something else?) Being very careful here as the solution becomes very hot.

4. EXTRACTION:
Add approx. as much xylen as the basified solution (please confirm the amount). Mix carefully. Then add this mixture to the separatory funnel, as shown in step 2, mix carefully (can I shake vigorously here aswell?), vent now and then. Put in hot water bath. Keep the upper liquid (xylene) and discard the lower one. Repeat 2 times.

5. SALT:
Add destilled water acified by acetic acid (pH 4 here aswell? He'll be using HCL for this step in the future after he built up some experience) remove the water keep it, discard the xylene. Repeat twice to get everything out of the xylene. What we have now is an acidic solution containing alkaloids. I pour it out on a wide surface to let it evap faster. Now that everything has evapped he scrapes the [insert alkalid name] acetate/hcl, voila!

Please add or edit something if necessary!

It would be very wicked if you could answer all his questions as he's a complete newb:>!

He'll be starting with this extraction in the beginning of next week, and add pics etc if anyone is interested.

Worth mentioning is that the alkaloid I'll be using for my first extraction is mesembrine (from sceletium tortuosum). Anyone with experience from this alkaloid?

 

[Noman]

It's a solid A/B extraction procedure.
I have no idea if it will work for kanna though.
Let us know how it goes.
Remember the first rule of experimental extracting - don't throw anything away.

 

[Kneegrow]

Thanks Noman for your quick reply!
I just got a few quick questions; when acidifying it on the 1st step, how long should it soak in the acidified liquid? Also when shaking the liquids in the separatory funnel could SWIM shake vigorously or does he have to shake gently (ofc he'll be venting now and then)? And the last one, as far is i've understood sodium carbonate is a weak base, should SWIM just pour some powder in to the acidic solution or should he first dilute it with some water and pour in?

Sorry if they were too long:>

 

[Shaolin]

1. Do you have any idea how your alkaloid acts under heat ? I would boil 3*60 minus in the acidification step.

2. Sometimes you can shake vigorously, sometimes you have to thread it like a baby. It's hard to predict such things but I would just invert it a couple of times but if you are not extremly unlucky even an emulsion that might form during vigirous shaking shall be dissolved when adding hot water/time/drumming on the glass.

3. I wouldn't be worried about local spikes with sodium carbonate. Also check the pKa if your sodium carbonate is strong enough. If you have no data available I would use the old school approach with NaOH and ph13.

 

[justine]

Defatting is useless with mhrb and as shaolin pointed out you should basify to ph 13 rather than 11.

 

[Granny]

3. I wouldn't be worried about local spikes with sodium carbonate. Also check the pKa if your sodium carbonate is strong enough. If you have no data available I would use the old school approach with NaOH and ph13.

Means that you should be able to add your sodium carbonate in it's pure form. Lye needs to be solved in water before adding. This'll keep the liquid you'll have to handle lower And you should be able to get around PH 12.
Just do a little test to figure out the possible problems before you throw it into your big bottle.

 

[endlessness]

as much solvent as the basified solution is way too much... Solvent should be like a tenth or something of the basified solution amount. Just keep repeating pulls till nothing more comes out

sodium carb yield if you pull with naphtha will probably be very low, so be sure to pull with xylene/limonene afterwards and/or add some NaOH at the end and pull again to see if more comes off (considering this is dmt.. dont know about mesembrine's pka and solubilities)

if you will pull from a dmt-containing plant, better salt your solvent with FASA/FASI/FASW and later convert to freebase, this way you dont need to defat at all

good luck

 

[Shaolin]

Keep in mind.

Worth mentioning is that the alkaloid I'll be using for my first extraction is mesembrine (from sceletium tortuosum)

 

[Kneegrow]

God damnit, So many replies so fast!

So NaOH is the preferable way to go with? And as for naphta for defatter, as I've read that it's the best choice for mesembrine.
Edit: sorry I just saw that you meant pulling and not defatting, it's defatted with naphta and pulled with xylene.

Thanks for the wicked replies btw!

 

[Kneegrow]

Okay just got some info about the alkaloid from merck;

Properties: Pale yellow oil. bp0.3 186-190°. [α]D20 -55.4° (CH3OH). Freely sol in alcohol, chloroform, acetone; slightly sol in ether. Practically insol in benzene, petr ether, alkalies.

Derivative Type: Hydrochloride
Molecular Formula: C17H23NO3.HCl
Molecular Weight: 325.83
Percent Composition: C 62.67%, H 7.42%, N 4.30%, O 14.73%, Cl 10.88%
Properties: mp 205-206°. [α]D20 -8.4° (CH3OH).

Derivative Type: (+)-Form
Properties: (Partially optically active). Pale yellow oil. [α]D20 +16.1° (c = 1.32 in CH3OH).

Derivative Type: (+)-Form hydrochloride
Molecular Formula: C17H23NO3.HCl
Molecular Weight: 325.83
Percent Composition: C 62.67%, H 7.42%, N 4.30%, O 14.73%, Cl 10.88%
Properties: Crystals from 2-propanol, mp 206.5-207.5°. [α]D20 +7.3° (c = 0.465 in CH3OH).

Derivative Type: (± )-Form
Properties: Colorless oil. bp0.07 178°.

Derivative Type: (± )-Form hydrochloride
Molecular Formula: C17H23NO3.HCl
Molecular Weight: 325.83
Percent Composition: C 62.67%, H 7.42%, N 4.30%, O 14.73%, Cl 10.88%
Properties: mp 179-181°.

So basically if I understand it correct, boiling point of the freebase is 186-190°? And the HCL's boiling point from approx. 170 to 207,5°? And are we talking fahrenheit or celcius? So if the alkaloids boiling point is over waters boiling point I should be able to boil it?

 

[endlessness]

ok look.. It doesnt say its solubility in xylene, but it says in benzene its only slightly soluble, so it might not be very soluble in xylene either (though this is theory, only practice can say for sure).

Maybe beginning with a dry tek would be more appropriate? Make paste with sodium carb or calcium hydroxide, pull with acetone, then proceed with purification?

BTW check this thread:

extracting pure mesembrine from sceletium tortuosum? - Other Psychoactives - Welcome to the DMT-Nexus

mesembrine freebase is an oil, so you need to salt it out if you want crystals. Personally I would try doing FASA on the dry pulls and see if fumarates crash out. Maybe dividing the extraction in half, with one half doing a xylene or acetone defat, then freebasing, then pulling with either of those and doing FASA, seeing if yield is different.

By the way, when you defat in an extraction, you should always use the same solvent for defat as you use for pulling, otherwise it wont be a good defat. You want to pull the impurities that dissolve in that solvent so that they are not there later, if you do with different solvents it kinda misses the point.

Anyways plenty of ideas there you can think about and that link with burnt's information which are very good. Good luck and tell us how it went!

 

[Kneegrow]

From what I've read (incl. from what burnt said) xylene/toluene is the best choice for pulling mesembrine, and as I've understood, he was successful with this approach, the reason I'm asking here is because I'm a complete newb and I wanted some clarification on the steps, I'll keep you updated with results

 

[Kneegrow]

Alright, I've made the extraction now waiting for evap, this is what I did;

added acetic acid and water to the plant material (100 grams ~1% alkaloid content) until the ph reached approx ph 4, defatting was kinda sloppy I first added naphta it kept turning yellow on every pull until I was out of naphta (about 4-5 pulls), So i decided to continue defatting with xylene (even though it would as I've read pull a small amount of alkaloids with it), did 2 pulls, it still did not turn clear so I decided to go on to the next step and re-do the defatting step later if necessary. As I do not have a separatory funnel I used a turket baster so I couldnt take that last milimeter of xylene layer, but I guess this wouldnt be a big issue since I'm going to add more xylene later after basification, anyways, I added sodium carbonate until ph reached approx 11 (note: as I have a cheap chinese ph meter these measurements are not exact), I now added xylene, gently turned the jar upside down for about 100 times (to avoid emulsion), eager to see the results I extracted some of the xylene
to another jar mixed with hydrochloric acid/water (ph approx 3-4), ending up with a white/cloudy solution that seems to contain the alkaloid salts.

Edit: I also got a very thin layer of xylene in the alkaloid/hcl solution, I hope that the xylene doesnt leave any toxic substances when evapping, or would it ?

I'll keep ya updated with pics as soon as evap is done

 

[taureanirishman]

Nice experimentation! Kanna is one of my favorites also so being able to have a starting point of doing a home extraction would be really cool...

Thanks to everyone else who's helping!!

 

[Kneegrow]

Okay SWIM ended up with a fine white/yellowish powder, scraped up with a razor, when SWIMS guinea pig tried to make a line with his card, it turned into to an unsnortable hard/oily solid mess, I guess this is due to the bad defatting process, could any1 confirm this? Should I re-do the defatting process?

 

[Kneegrow]

anyone?

 

[taureanirishman]

according to endless' post mes freebase is an oil, so it sounds like you need to do a salting process(no idea how, just restating what I read) if your guinne wants to use a tooter. Personally I'd see what it's like to do a vapor hit of it... Might make an interesting thing to combine with jimjam....

 

[Kneegrow]

if you read above you'll see that I salted it out with diluted hcl (ph ~3.0), anyways now I defatted the crap out of it with naphta (about 6-7 pulls) and I'll wait for evap n see

 

[Kneegrow]

Got almost the same result if not the same, a white yellowish fluffy powder, as soon as SWIM put a tiny bit on SWIMS fingertip it turns into a brownish sticky oil and it smells like chlorine, could this be due to the HCL acid SWIM used for salting out? What should SWIM do? Should SWIM wash it out with acetone or something?

Edit: I also forgot to mention that the acidic solution probably had some traces of NP solvent in it as it had a slight NP solvent smell (there were no visible NP layer), but this shouldnt be a problem when evapping as SWIM repeated the defatting step approx 10 times

 

[Kneegrow]

Could it have something to do with heat? When SWIM evapped it he put the glass tray on an eletric stove on weak setting.