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FASI with P. aquatica AQ1; does this look / sound right? Options
 
Jagube
#1 Posted : 6/25/2019 11:29:14 PM

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I'm extracting my garden-grown grass. Roughly 180 g fresh grass, which is really only a handful and was harvested from maybe 4 sq. ft of garden space of sparsely planted grass (which will get denser with time).

I boiled it, reduced it, based with lime, dried and pulled with IPA.
The material I was pulling from with IPA was a very sticky goo. The IPA turned amber.

Now I'm doing FASI precipitation for the first time in my life and it's clouding like crazy! I'm loving this tek as it's so easy to see what's going on, how much of what to add and when to stop. And in the process I've only used vinegar, lime, IPA and fumaric acid. No sticky oils or toxic chemicals, and the only sticky material is the based and dried matter to pull with IPA from. And I think I can reuse the IPA pulls in further pulls.
Also removing the IPA pulls from the basic goo was super easy as the goo was so sticky there was no need for decanting or filtering, I was able to just pour it off.

I thought the fumarate crystals would be large crystals, but they're a light, clouding powder and form a fluffy sediment. Will they form larger crystals later? And if they are to remain a fluff, what would be the best way to get them out of the IPA: basting it off and evaporating the last bit of IPA, or running it through a coffee filter?

I'm still adding drops of FASI, watching the clouding and letting it settle. I'll report the final yield. I'm interested in the salt form as it's for oral administration, and if I understand correctly the fumarates will be full-spectrum, which is also what I'm after (for one, I reckon the grass contains roughly as much DMT-n-oxide as n,n-DMT).

There is also the possibility that the precipitate is not DMT but some other alkaloid, but assuming it's AQ1 (which it seems to be) I don't know what else it could be?
 

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Jagube
#2 Posted : 6/26/2019 11:07:38 AM

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I didn't want to filter it as the precipitate looked so tiny I thought it might pass through the filter, so I decanted most of the IPA off and transferred the precipitate with a bit of the amber-colored IPA into the evaporating dish.

I understand the IPA residue will contaminate my product (with fumaric acid and whatever else the IPA may have pulled that's not an alkaloid), but since this is for oral ingestion I'm not too worried. I guess I can always wash it with fresh IPA, but that would be a waste of IPA and might incur some product loss, and for my purpose it's not really necessary.

I can see some crystals in the dish, they're white and look like freebase DMT from freeze-precipitated MHRB naphtha pulls.

But at the lower side of the dish, where the IPA is, the product is forming clumps.

Photo attached. I edited it to improve the contrast, as a result the color came out a bit more yellow when in reality it's more amber.

The whole thing smells like toffee, with a hint of biscuit and maybe even anise.
I can't wait to weigh and bioassay it.
Jagube attached the following image(s):
evap.jpg (607kb) downloaded 172 time(s).
 
endlessness
#3 Posted : 6/26/2019 12:07:12 PM

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I would definitely try filtering that, worse that happens is it doesnt work and you retrieve your product below your filter. Ideally it stays on top of filter and will have much less contamination.

Did you add the FASI very slowly? The slower, the nicer crystals.

Also, I'd be careful with bioassaying phalaris extract without at least some sort of testing, whether reagent or TLC or similar. Is that a possibility?

Otherwise this is also a possibility, though results would be slow, at least it would be interesting knowledge for the future.. Want to send the lab some?
 
Jagube
#4 Posted : 6/26/2019 3:02:36 PM

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endlessness wrote:
I would definitely try filtering that, worse that happens is it doesnt work and you retrieve your product below your filter. Ideally it stays on top of filter and will have much less contamination. [..]

Also, I'd be careful with bioassaying phalaris extract without at least some sort of testing, whether reagent or TLC or similar. Is that a possibility?

I've drank crude tea from this grass in the past. It was unpalatable and unkind to the stomach, but active (a DMT feel with pastel colored visuals / visions).

The upalatability and bad stomach effects had motivated me to extract the grass, and this is my first extraction beyond crude tea that seems to have worked.

Next time I might try filtering and see how that works and whether it's more practical.

My toolkit doesn't include reagents or TLC (yet).

I'm not that worried about potential gramine content that might have slipped in with the IPA. If this is indeed AQ1, it shouldn't contain any. But in any case, my crude tea bioassay didn't seem to produce any toxic effects, apart from the stomach discomfort which I don't think was of alkaloidal origin.

So I'm happy to bioassay the amber goo, which seems to be a mix of fumarates and oils.

endlessness wrote:
Did you add the FASI very slowly? The slower, the nicer crystals.

Thanks. I added it dropwise, but perhaps not slowly enough. Also the volume of my IPA was small (100 ml combined pulls), which may have produced smaller crystals.

endlessness wrote:
Otherwise this is also a possibility, though results would be slow, at least it would be interesting knowledge for the future.. Want to send the lab some?

I was aware of that offer, thanks for the reminder. I'm also extracting my garden-grown Acacia floribunda (shrub form), so when that's ready, maybe I can send in both the Phalaris and the Acacia?

Would the fumarates partially contaminated with evaporated IPA be suitable, or would they have to be filtered?

Attached picture of the sticky product after scraping what I managed to scrape.
Yield: 440 mg. It's hard to tell how much of it are the fumarates and how much are impurities.
Jagube attached the following image(s):
evapped.jpg (103kb) downloaded 155 time(s).
 
endlessness
#5 Posted : 6/27/2019 9:44:47 AM

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Jagube wrote:

I've drank crude tea from this grass in the past. It was unpalatable and unkind to the stomach, but active (a DMT feel with pastel colored visuals / visions).


You're a brave man, thanks for sharing your experience. But please be careful, different phalaris species have a variety of compounds, not only gramine, which we have no clue about their toxicity, short and long term. But yeah, definitely extracting is probably a better idea than consuming a straight tea.. Either way indeed I'd love to help that get tested. You can indeed send even with the evapped IPA contam, no worries. And sending that together with the acacia sounds good.

How much phalaris did you extract to get those 400+mg ?

Lets keep in touch!

Be well!
 
Jagube
#6 Posted : 6/27/2019 8:32:11 PM

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endlessness wrote:
You're a brave man, thanks for sharing your experience. But please be careful, different phalaris species have a variety of compounds, not only gramine, which we have no clue about their toxicity, short and long term. But yeah, definitely extracting is probably a better idea than consuming a straight tea.. Either way indeed I'd love to help that get tested. You can indeed send even with the evapped IPA contam, no worries. And sending that together with the acacia sounds good.

How much phalaris did you extract to get those 400+mg ?

I know P. arundinacea can be highly variable, but this is definitely P. aquatica, which appears to be less variable, and it's likely to be AQ1, but the jury is still out on that.

The starting plant material was ~180 g fresh grass. I didn't only harvest the upper parts of the blades, which are supposed to be the most potent; I trimmed the grass indiscriminately, including the stalks, to make it easy and quick. Also I didn't harvest it in the morning when it's supposedly the most potent, but in the afternoon. And I didn't do any stressing to maximize its potency. It was harvested after a period of rain and a day after fertilizing with nitrogen.

I think I messed it up a bit. I bioassayed 63 mg of the goo, 10 minutes after 200 mg fb harmine (likely contaminated with harmaline) and 95 mg fb THH (which had recently been accidentally exposed to heat and might have partially converted back to harmaline). Considering the DMT fumarate to DMT freebase weight ratio of 1.31, 63 mg *pure* DMT fumarate would represent 48 mg fb DMT.

I only felt very faint DMT effects. I also felt waves or pulses of energy and it had an electric, zesty quality, but it's hard to say if that was of tryptamine or beta-carboline origin. My conclusion was that the IPA contamination must have been rather significant.

180 g fresh grass is equivalent to 18 g dried grass, which assuming the optimistic 1% DMT content of AQ1, would contain 180 mg DMT. The 440 mg goo (which may not even have contained all the purported DMT, as I probably didn't add enough FASI - the clouding takes long to settle and I was impatient) further confirms a high IPA contamination.

I decided to clean it up a bit (for the analysis, but also to better gauge a dose), so I put the goo back in the amber IPA and on the magnetic stirrer. Some of it dissolved, but some goo stayed at the bottom and proved very sticky. I transferred the IPA into another jar and added more FASI to precipitate again (and possibly more). Then I added a bit of water to the sticky goo (with IPA removed) and it dissolved immediately. I'm currently drying the water with the goo in it, as well as the fumarate crystals from the other jar. I guess I should have filtered the crystals at the beginning to begin with. The reason I was reluctant to filter is I thought it was a relatively small amount and a lot of product would be lost to the filter. But come to think of it, since the fumarates are soluble in water, I can always wash the filter with water and evaporate the wash to retrieve them.

So what I have now is water with fumarates and sticky stuff dissolved in it drying, as well as fumarate crystals lightly contaminated with IPA evaporating.

The crystals are cleaner (they're off-white, like the THH from harmaline from my rue extractions), so I'll send those rather than the sticky stuff. You said 10-20mg is plenty, I definitely have more crystals than that (probably by an order of magnitude), so that's sorted Thumbs up And I'll report the yield once it's dried. But I don't think it's the complete yield. I did another (4th) IPA pull and it clouded upon adding FASI, so there may still be more alkaloids in the basic goo, but probably not much.

The acacia is up next. I'm still drying the goo (to pull with IPA from), which comes from limonene / sunflower oil pulls, salted with vinegar, reduced and basified with calcium hydroxide. The residual oils may be the reason it's drying so slowly.
 
grollum
#7 Posted : 6/28/2019 1:22:58 PM

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I am really curious what the analysis will show. Good work.
 
Jagube
#8 Posted : 7/1/2019 3:18:37 AM

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endlessness wrote:
But please be careful, different phalaris species have a variety of compounds, not only gramine, which we have no clue about their toxicity, short and long term.

Are there any alkaloids (grass related or not) that cause long term negative effects after one-off exposure?
Long term toxicity generally comes from things that stay in the body (e.g. heavy metals, asbestos etc.). Alkaloids are organic molecules and, generally, get metabolized relatively quickly. But I may be wrong.

Do we have any data on whether gramine or other potentially undesirable alkaloids precipitate in FASI as fumarates?

I weighed the off-white, powdery product; it was a nice 185 mg.
The sticky, IPA-contaminated goo (or what I managed to scrape off anyway) weighs 335 mg, although that doesn't indicate much as the level of contamination is unknown.

I was encouraged by these results and bioassayed the powder. I took 180 mg THH, followed by 200 mg harmine 30 minutes later, and ~60 mg of the powder another 10 minutes later. I was expecting strong DMT effects, but the effects were very faint and I'm not sure how much of it was the harmalas. It tasted sour, but in a nice way. I don't think DMT fumarate is supposed to taste sour, so I wonder if it was residual fumaric acid from solution that stayed in the product after drying?
I had realistic quality visions (as opposed to abstract visuals, which were absent), but surreal in their content, e.g. my mom riding a motorbike. They engaged my attention, but didn't last long (maybe 30 minutes?) It could have been the harmalas to a large extent, although IIRC there was some color.

Eventually I ended up vaping some DMT from MHRB to make the most of the harmala-ified state, and had a good, long-lived experience. Eight hours later I'm still feeling it.

My conclusion is that the powder is not DMT fumarate for the most part, although it likely contains some DMT.

I'm hoping to extract the acacia and send both samples this week.

Edit: The basic goo I was pulling the Phalaris with IPA from is very water soluble, but not IPA soluble at all. I'm wondering if the goodies may have been trapped in it? If I re-dissolve it in water and run through a coffee filter, will the freebase goodies stay in the filter?
 
Jagube
#9 Posted : 7/1/2019 3:39:28 PM

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I added water and dissolved the goo. Then topped up calcium hydroxide as the pH dropped to the 8's.

It's now settling and there is a white-ish precipitate at the bottom, with brown supernatant. Looks very much like a harmala base extraction. Maybe that's where the DMT is?

I'll allow it more time to settle and become more compact, then decant the supernatant off and maybe filter through a coffee filter to separate the water-solubles from the insolubles, and dry the latter. Then pull the latter with IPA for FASI, and the former with limo/sunflower just in case any goodies made it through the filter.
Jagube attached the following image(s):
phala b water.jpg (407kb) downloaded 99 time(s).
 
Chimp Z
#10 Posted : 7/1/2019 4:02:56 PM

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Jagube you're doing great work! I always wondered about FASA and FASI Phalaris extracts and
if I should pick some FA up.
Do you have acetone or naphtha available in your area?
I would recommend using those solvents and performing defats before adding base.
Cool
Also if you're in control of cultivating this grass, let it grow back, cut it back again and the 2nd regrowth should be more potent. You might have a little less grass to work with though...
Love
http://www.flockandherd....halaris-staggers-II.html
 
Jagube
#11 Posted : 7/1/2019 5:11:27 PM

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Chimp Z wrote:
Do you have acetone or naphtha available in your area?
I would recommend using those solvents and performing defats before adding base.
Cool
Also if you're in control of cultivating this grass, let it grow back, cut it back again and the 2nd regrowth should be more potent. You might have a little less grass to work with though...

Thanks Chimp Z.

Yes, both acetone and naphtha are available here, and I have naphtha but would have to order acetone.

I've never done a defat, I guess I've been reluctant to use a solvent and not be able to re-use it.

Why do you think acetone would be better than IPA? Downwardsfromzero has hinted acetone might react with calcium hydroxide in a condensation reaction, but from what I understand this hasn't been confirmed. Also if I understand correctly, acetone absorbs atmospheric moisture more readily and needs to be dried with magnesium sulphate, whereas 99.9% IPA is good as it is.

The precipitation in the last posted picture looks like a very nice, efficient separation (a'la rue tea basing), so maybe de-fatting is not needed (or did my initial IPA pulls effectively defat it)? I'm curious as to what the precipitate is (part of it may be calcium hydroxide, but it looks to be much more than the amount of Ca(OH)2 I added). If there are any goodies in this material, they must be either in the supernatant or the precipitate.

I might vape some of the precipitate for a quick test, calcium hydroxide contamination shouldn't be an issue with vaping, right? As its boiling point is quite high.

I am in control of cultivating this grass, not sure which regrowth it was that I harvested the material from. I thought the 2nd regrowth was supposed to be the most potent in the spring and now this grass is supposed to be entering summer dormancy.
 
Jagube
#12 Posted : 10/23/2019 8:03:09 PM

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Now I'm confused.

I pulled my phalaris with sunflower oil / limo, dried it, based with ammonia solution, dried again, then pulled with IPA and did FASI on that.

The precipitate is a white / off-white powder, but, based on bioassays, it doesn't seem to contain much if any DMT.

It was my understanding that FASI is fairly selective for DMT; what's not DMT, shouldn't precipitate.

Any ideas what it might be? It's water-soluble, somewhat bitter and sour.

I have reasons to suspect it's some beta-carboline, because when I take it with harmine and THH, the harmala (or harmala-like) effects seem stronger than what the harmine and THH would account for.

Do we know of any other alkaloids that precipitate in FASI?
 
endlessness
#13 Posted : 10/23/2019 9:46:32 PM

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Why dont you at least get some reagents or look into TLC?. You will be able to answer a lot of questions about your specific extract.. Even if people can speculate and give you informed ideas, still nothing beats testing.
 
Triglav
#14 Posted : 6/29/2020 11:08:33 AM

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Very good thread with great information! Thanks a lot for all the work! Thumbs up

Some months had passed since the last post in the thread. Is there are any new information available now regarding this Jagube ?
 
Jagube
#15 Posted : 6/29/2020 4:06:34 PM

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The FASI precipitate didn't seem to contain any DMT.

I have yet to do a successful FASI; I've recently done it on MHRB and some IPA washes of my GVG, and again, the FASI precipitates don't contain DMT (not in noticeable amounts anyway) as far as I can tell: 50mg with harmalas didn't produce any DMT effects.
 
Triglav
#16 Posted : 6/29/2020 5:31:02 PM

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Jagube wrote:
The FASI precipitate didn't seem to contain any DMT.

I have yet to do a successful FASI; I've recently done it on MHRB and some IPA washes of my GVG, and again, the FASI precipitates don't contain DMT (not in noticeable amounts anyway) as far as I can tell: 50mg with harmalas didn't produce any DMT effects.


I see. Interesting.

So the lack of DMT in the FASI phalaris extract you've made is most likely not because there was no DMT in the grass but because you had failed to do the FASI successfully ? I presume there should be DMT in the in the MHRB you worked with.
 
Jagube
#17 Posted : 6/29/2020 7:42:51 PM

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Triglav wrote:

So the lack of DMT in the FASI phalaris extract you've made is most likely not because there was no DMT in the grass but because you had failed to do the FASI successfully ? I presume there should be DMT in the in the MHRB you worked with.

Yes. And of course there is DMT in the MHRB; naphtha with freeze precipitation yielded 1.4% until I quit doing further pulls.
 
 
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