Chaliponga

[Noman]

So my friend has started his third chaliponga extraction with an eye towards investigating whether it's just MHRB that needs high (12+) pH to avoid emulsions and how well a citrate separation works for NN DMT and 5MEO.
The leaf was crushed and cooked in his usual 1/2 vinegar water mix twice and then twice more in plain water, the extracts combined, reduced by 2/3, defatted three times with xylene, basified with lye to pH 9.5 and extracted with heptane.
The heptane was placed in the back of his freezer and two days later is clear with (by his estimate) 150mg of very fine white particulate floating around.
There was very little emulsion to deal with, what there was broke quickly with a bit of heat and a few runs through the sep funnel.
What precipitated out did not clump up or stick to the sides of the jar as is commonly the case with MHRB.
After the first pull, he added more heptane to the solution and agitated three times and let it sit.
Now, two days later, the heptane has a good bit of something moved up into it (very cloudy) and the basified solution has a lot of chunky particulate in the bottom half.
The color has changed from brown to brick red too.
He's looking for ideas on how to proceed, especially with the basified solution.
Pull off the second heptane pull and try to kick whatever is in it out?
What are those chunks in the bottom? Should he try pulling with a less selective solvent and see if the chunks dissolve into that?
Should he basify further like his MHRB experience tells him?

 

[lemmy]

a wee bit of topic here noman but i was just wondering about the 1/2 vinegar water mix.do you allways use this amount of vinegar.when making aya brews ive allways found 30ml per littre of water to be more than enough.

 

[Noman]

Alright.
That first pull yielded shit.
Whatever was in there never formed anything solid enough to get trapped in the filter.
He separated his second pull
(subsequent agitation had it forming emulsions that would settle out)
and combined it with the heptane from his first pull.
Then he shook the shit out of the aqueous solution
and quickly divided it in two.
One half he left alone and the other half was basified to pH 12.
Half of the combined heptane was added to each jar
and the jars were agitated periodically over the course of several hours.
Here they are next morning:

The one on the left is the one taken to pH 12.
The one on the right left at pH 9.5.
Its weird how much this stuff looks like an MHRB extraction once you get to this point.
Even the color...
Anyway -
he separated them both and broke the emulsion on the right jar
and evaped them both
and got yellow oil.
Maybe 100mg - too goopy and too little to really bother weighing right.
About 4X as much from pH 12 as pH 9.5.
He redissolved it in heptane and soaked it up with a gram and a half of 7X salvia he'd already laced with NN.
Interesting times ahead.

Before he separated the jar on the right though
he sucked the particulate matter off the bottom.
It is now dry(ish)
and he is about to rinse a third of it
in some warm heptane
and a third in warm acetone.
If there's precipitated freebase in there
it should dissolve into one of the two
or both.
Yeah?
Thoughts on what to do with the other third?

 

[Big Inhale]

We definitely need a trip report on that salvia/spice you got there. That makes me jealous.

 

[Observant]

We definitely need a trip report on that salvia/spice you got there.

WORD! :lol:

 

[Noman]

Why be jealous? Dissolve a little freebase in the solvent of your choice, throw in some salvia extract, and let it dry.
My friend likes about 10:1 - salviaMT using 7X salvia but since mileage varies so much with each of these (my friend is an extreme lightweight with salvia but has a normal DMT tolerance), one should tune their blend to suit them. Just remember that they are extremely synergystic - 4X I'd say, but my friend prefers the combined trip over either of the two solo unless he's after a full balls DMT breakthrough.

Anyway, so he washed the particulate in hot acetone and heptane, filtered them and dried each solvent.
The acetone wash dried down to an oily red residue. A small taste test told him that it did contain DMT of some kind.
The heptane wash yielded nothing.
Weird, why would the alks be soluable in acetone and not heptane? Would they have precipitated out as salt? I didn't think the salt was soluable in acetone anyway.
So I'm going to have him filter out the rest of the precipitate for further experimentation, combine the filtered solution with the pH 12 solution and take that up to 13 and try extracting from there with naptha as well as heptane in case there's something about chaliponga extract that's insoluable in heptane.

Still looking for thoughts on what to do with this precipitate.

 

[Infundibulum]

10:1 - salviaMT

Exactly!

 

[69ron]

So my friend has started his third chaliponga extraction with an eye towards investigating whether it's just MHRB that needs high (12+) pH to avoid emulsions and how well a citrate separation works for NN DMT and 5MEO.
The leaf was crushed and cooked in his usual 1/2 vinegar water mix twice and then twice more in plain water, the extracts combined, reduced by 2/3, defatted three times with xylene, basified with lye to pH 9.5 and extracted with heptane.
The heptane was placed in the back of his freezer and two days later is clear with (by his estimate) 150mg of very fine white particulate floating around.
There was very little emulsion to deal with, what there was broke quickly with a bit of heat and a few runs through the sep funnel.
What precipitated out did not clump up or stick to the sides of the jar as is commonly the case with MHRB.
After the first pull, he added more heptane to the solution and agitated three times and let it sit.
Now, two days later, the heptane has a good bit of something moved up into it (very cloudy) and the basified solution has a lot of chunky particulate in the bottom half.
The color has changed from brown to brick red too.
He's looking for ideas on how to proceed, especially with the basified solution.
Pull off the second heptane pull and try to kick whatever is in it out?
What are those chunks in the bottom? Should he try pulling with a less selective solvent and see if the chunks dissolve into that?
Should he basify further like his MHRB experience tells him?

The way you put that extraction together, you’re going to get very poor yields at pH 9.5.

Noman, that type of extraction at pH 9.5 is going to work better if you use DCM, ether, or chloroform. DMT is very poorly soluble in heptane. With heptane you need to force the DMT into it by either heating the heptane or nearly saturating the water with some kind of base. If you use sodium carbonate instead of sodium hydroxide you can reach the saturation point at a lower pH. But why not just use DCM? DCM extracts DMT like a magnet extracts iron from sand. It holds a ton of DMT. It’s perfect for extracting DMT.

All of SWIM's highly successful extractions at pH 8.5-10.5 use DCM as the non-polar solvent, and sodium carbonate as the base, not heptane or naphtha or sodium hydroxide. That’s a different ballgame.

SWIM has extracted many times from chaliponga using ph 3 water (with citric acid), defatting with DCM, adjusting the pH to 9.5 with sodium carbonate, extracting into DCM, and then drying and freeze precipitating in heptane. When dissolving the alkaloids in the heptane for freeze precipitating, the yellowish junk that doesn’t dissolve in the heptane is very potent, stronger than DMT and you want to keep it. But if you used heptane as the extraction solvent, you won’t get that extra potent stuff in your product and so you’re wasting your money.

I think attempting to extract from chaliponga like it’s mimosa is probably a bad idea. There are some active alkaloids in chaliponga other than DMT which are almost insoluble in heptane. You want to use a tech that works for something like Yopo that isn’t so DMT centric. That basically means using a solvent like DCM, ether, or chloroform, and not bringing the pH up too high. Some of the alkaloids in chaliponga seem to be sensitive to a high pH. Also, if using heptane, you’re going to exclude some very potent unknown alkaloids from your extraction. SWIM knows, he’s played around with chaliponga for quite some time now. It’s similar to Yopo. Like Yopo, if you attempt to extract with heptane, you’ll get really poor yields and lost most of the active alkaloids. Also pH 13+ with Yopo destroys most of the alkaloids. This is also the case with chaliponga, but not so severe.

 

[Noman]

Thanks Ron.
Except every time you reply to one of my posts, my friend ends up with about a million more things to try out.
I guess I'll have to get him to get hold of some DCM and check that out - should ether or chloroform work equally well? They would be a little easier to procure.
I get what you're saying about other alks in the chaliponga not extracting into heptane or naptha, but why wouldn't whatever DMT that's in there get pulled just like from mimosa? He's getting marginally more at pH 13 than the almost nothing he gets from pH 9.5, but it's still just a tiny bit of some (albeit VERY potent) oil.
Also, I just can't agree that pH 13 extraction works better because of the solution being saturated. There isn't enough lye in there to come even close to saturating the solution and experiments that he's done with lower pH solutions saturated with salt resulted in the same poor yields. More likely, IMHO, is that the alks are more soluable at the higher pH - at least more soluable in heptane or naptha, once he gets some DCM he'll see if that makes the difference.
The precipitate experiment seems to support this - did you see that post? It's in the middle of this thread. The precipitate at pH 9.5 definitely containd freebase DMT that is soluable in acetone but not heptane. Something definitely changes when one goes above pH 11 or 12 and the solution changes from cloudy milkshake to slippery black - the precipitate disappears. It seems like this must have something to do with the change in soluability. He has a good bit of this precipitate now and once he gets a better collection of solvents together he'll do some more testing on that.
He still has plenty of chaliponga left so he'll be playing around with a few things in the future. I'll have him try what you suggest, a few different other solvents, maybe a solvent (IPA?) extraction first followed by an A/B, maybe an acid extraction cooked down with calcium hydroxide added followed by an acetone wash like with yopo.
Keeping in mind of course that this batch of chaliponga could just have very little alkaloid content.
All part of the fun eh?
Thanks for the feedback, keep it coming.

 

[69ron]

Thanks Ron.
Except every time you reply to one of my posts, my friend ends up with about a million more things to try out.
I guess I'll have to get him to get hold of some DCM and check that out - should ether or chloroform work equally well? They would be a little easier to procure.

Yes ether or chloroform should be almost as good as DCM.

I get what you're saying about other alks in the chaliponga not extracting into heptane or naptha, but why wouldn't whatever DMT that's in there get pulled just like from mimosa? He's getting marginally more at pH 13 than the almost nothing he gets from pH 9.5, but it's still just a tiny bit of some (albeit VERY potent) oil.

Most leafy plant material oxidizes really fast and so by the time the plant gets purchased by the user, a lot of the DMT has oxidized to DMT N-Oxide. I’m sure that’s why the yield is so low. DMT N-Oxide is not soluble in heptane or naphtha and by using one of those solvents you exclude that highly important alkaloid from your extraction.

Also, I just can't agree that pH 13 extraction works better because of the solution being saturated. There isn't enough lye in there to come even close to saturating the solution and experiments that he's done with lower pH solutions saturated with salt resulted in the same poor yields. More likely, IMHO, is that the alks are more soluable at the higher pH - at least more soluable in heptane or naptha, once he gets some DCM he'll see if that makes the difference.

I don’t know what to say about that Noman. SWIM always uses pH 9.5 with DCM and gets great yields. SWIM is not sure what exactly the sodium hydroxide is doing, but SWIM is sure it has nothing to do with the pH. SWIM believes the sodium hydroxide is pushing out the DMT much the way sodium carbonate can push out isopropyl alcohol and acetone from water. It’s not a pH thing but rather a chemical concentration thing. DMT is apparently not very soluble in sodium hydroxide. It’s not the pH. SWIM is sure of that. The pKa of DMT is too low for it to be related to pH.

The precipitate experiment seems to support this - did you see that post? It's in the middle of this thread. The precipitate at pH 9.5 definitely containd freebase DMT that is soluable in acetone but not heptane.

Noman, I’m sure that is probably freebase DMT N-Oxide (or 5-MeO-DMT N-Oxide) and not freebase DMT. Chaliponga has a lot of DMT N-Oxide in it. Freebase DMT N-Oxide is soluble in acetone, but not in heptane. Freebase DMT is soluble in both.

Keep in mind that this is not Mimosa. Chaliponga has a lot of other alkaloids other than DMT. It usually has lots of N-Oxides in it.

Something definitely changes when one goes above pH 11 or 12 and the solution changes from cloudy milkshake to slippery black - the precipitate disappears. It seems like this must have something to do with the change in soluability. He has a good bit of this precipitate now and once he gets a better collection of solvents together he'll do some more testing on that.
He still has plenty of chaliponga left so he'll be playing around with a few things in the future. I'll have him try what you suggest, a few different other solvents, maybe a solvent (IPA?) extraction first followed by an A/B, maybe an acid extraction cooked down with calcium hydroxide added followed by an acetone wash like with yopo.
Keeping in mind of course that this batch of chaliponga could just have very little alkaloid content.
All part of the fun eh?
Thanks for the feedback, keep it coming.

SWIM now loves the process of extracting more than the products they produce. It is a lot of fun, especially when there are mysteries to solve. The DMT and pH 13 thing is one mystery that SWIM is trying to tackle. It makes no scientific sense to SWIM, however many people do get better yields at that pH when using naphtha, heptane, or hexane as their non-polar solvent in A/B extractions. The pKa of DMT is 8.68. At pH 9.68 90% is freebase. At pH 10.68 99% is freebase. At pH 11.68 99.9% is freebase. At pH 12.68 99.99% is freebase. At pH 13.68 99.999% is freebase. There’s very little difference between pH 9 and pH 13, considering you need to pull 3 times anyway. SWIM uses DCM and found better yields at pH 9.5 than 11 or above. The main reason is that some of the other plant alkaloids get destroyed at pH 11 and above.

Noman, why would you think pH would have anything to do with this? At pH 13.68 99.999% is freebased. At pH 9.68 90% is freebased. So at best you could maybe get that extra 10% at pH 13. But if doing 3 pulls you should get all of it even at pH 9.68. Which is the case when using DCM, but not when using heptane. WHY?

 

[Noman]

Noman, why would you think pH would have anything to do with this? At pH 13.68 99.999% is freebased. At pH 9.68 90% is freebased. So at best you could maybe get that extra 10% at pH 13. But if doing 3 pulls you should get all of it even at pH 9.68. Which is the case when using DCM, but not when using heptane. WHY?

Well, my friend is obviously going to have to do quite a bit more research using various bases and NP solvents.
Thus far, he's only worked with lye, ammonia, naptha, xylene, toluene, and heptane.
It's simplistic to be sure, but I think pH has something to do with it because emulsions aside, he gets better yields at higher pH. Better as in 90% more rather than 10% more. Maybe it's not pH, maybe it's concentration or something else, but at any rate the alks don't seem to become soluble in heptane or naptha until the pH gets up above 12.
I'm an empiricist - I really know fuck all about the chemistry underlying all this.
Anyway, it seems that a pH 10 extraction is in order using chloroform for the NP.
I'll have him start with some MHRB with a known alk % before he works with the chaliponga.
So the chaliponga is going to likely be a lot of NN oxide, right?
That should extract as an oil unless he reduces it with zinc first, shouldn't it?
Will the reduction affect those unnamed alks in the chaliponga too?
Well, he'll see but all these experiments are producing products needing a bioassay at a much faster rate than my friend likes to dose.
Like you said, the craft is just as rewarding and consciousness changing as the tripping.
More sometimes.

 

[69ron]

Yeah, the DMT N-Oxide is going to be an oil.
Keep in mind that the 5-MeO-DMT N-Oxide is also an oil. The mixed oil is REALLY STRONG. BEWARE. It's much stronger than DMT. At least 3-5 times stronger. One full inhalation of it will blow most people out of their minds.

I don't know how effective reducing with zinc is prior to extraction. I've only seen it done after extraction. The reducting with zinc will affact all the N-Oxides in chaliponga. There's DMT N-Oxide and 5-MeO-DMT N-Oxide in there and probably other unknown ones. The plant hasn't been studied that much.

After making an extract with DCM, ether, or chloroform, it's going to be an oil because of all the N-Oxides present. You can reduce it with zinc with the standard zinc reduction procedure if you like. Then you’ll get dry freebase crystals. It’s a pain though. Another option is that you can add calcium carbonate to the oil as is to make it dry enough to pour and measure out doses. The ratio of calcium carbonate to oil needed is 10:1. SWIM usually does this so that he can measure out the yield of oil and use it AS IS. He normally uses it sublingually. It produces an LSD-like effect that way. It's VERY NICE. It's one of SWIM's favorite psychedelics. All it takes is 5-15 mg of oil under the tongue for 5 minutes and you’re tripping very nicely. It’s a beautiful experience.

 

[Noman]

I don't know how effective reducing with zinc is prior to extraction. I've only seen it done after extraction.

After making an extract with DCM, ether, or chloroform, it's going to be an oil because of all the N-Oxides present. You can reduce it with zinc with the standard zinc reduction procedure if you like. Then you’ll get dry freebase crystals. It’s a pain though.

Couldn't this oil have the NN separated with a warm heptane wash leaving freebase crystal NN and yellow n oxide oil?
Also, I'm thinking that a chloroform extraction of MHRB would result in jungle spice being present in the oil. Is n oxide soluable in xylene? If not, that would be the way to separate the jungle from the oxide.

 

[69ron]

I don't know how effective reducing with zinc is prior to extraction. I've only seen it done after extraction.

After making an extract with DCM, ether, or chloroform, it's going to be an oil because of all the N-Oxides present. You can reduce it with zinc with the standard zinc reduction procedure if you like. Then you’ll get dry freebase crystals. It’s a pain though.

Couldn't this oil have the NN separated with a warm heptane wash leaving freebase crystal NN and yellow n oxide oil?

Yes. SWIM does that all the time. Mix the oil with warm heptane and DMT and 5-MeO-DMT will dissolve in the heptane and the N-Oxides and other stuff stays behind as yellow oil on the bottom of the jar. Pour off the heptane and freeze precipitate it in another jar. That way you have pure DMT and 5-MeO-DMT crystals and your N-Oxides and other goodies left behind as yellow oil.

Also, I'm thinking that a chloroform extraction of MHRB would result in jungle spice being present in the oil. Is n oxide soluable in xylene? If not, that would be the way to separate the jungle from the oxide.

Sorry, I don’t know if DMT N-oxide is soluble in xylene or not. I know it’s soluble in DCM, ether, acetone, chloroform, alcohol, and insoluble in naphtha, heptane, and hexane.

 

[Infundibulum]

SWIM can affirm from his experience that DMT n-oxide is soluble in xylene and insoluble in naptha!

 

[Noman]

SWIM can affirm from his experience that DMT n-oxide is soluble in xylene and insoluble in naptha!

Good to know.
Half of the reason for my incessant questions is sheer laziness
on the part of my Antarctican friend
not wanting to test things
that somebody else has already tested.