💎 THCA on deckđŸ”„ 10 g MOQ

Hempire Building Hemp Outlet
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Thanks, I hope you can appreciate my questions
as It does seem indeed an number of ways to “crack that code”
And you do understand my questions
so I appreciate that detail as well
as there are a number of ways to come up with 99% COA as proof of knowing what you are doing
but nice to see you openly discuss the 90s% number in bulk runs. Yes looking at those numbers that include the other acids and no neutrals, gives me a much better idea of the process. (Low level of D9 is questionalble)

If you see the recent work by Sambo Creek posted on 4200, the finest fractions with “ideal trichomes” give you 73% THCA 
boom, a very nice starting material.

Do you use a particular step to “force” the cannabinoates into the cannabinoic acid form? There is one academic paper that discusses this. If not, I do not know how anyone can think they have cannabinoic acid, pure state.???
Thus my question on salts.

Best regards,

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Ive seen mechanical water extracts with over 76% thca
 and not with premium flower


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You mean trichomes? Correct
.yes I would think there is a variation of these factors 
73-76 ???

Certainly the luck of the day
or what corner of the field the biomass comes from

Point is there is a bit of variation
when it comes to COA’s of mechanical trichomes
.but even the finest sifts and cuts have a limit. Are you talking wet? COA , air dried, or hard vacuum freeze dried
?
And are you talking total cannabinoids or total THCA in marijuana strains
? I’d really like to get a consensus number for everyone to rely on
but obvious water content needs to be standardized.

It is really more about possibilities of carboxylic acid /anion complexes, as the higher the number , it eliminates certain complexes on a mole basis after taking terpenes, lignins and other “hull” components into account.

Yes and a pseudo one step base-water extraction.moves that number to 90 (no decimal) % or so 


High affinity directed Self assembly into crystals can move that number to 98% plus


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Ok
tq

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The cannabanoids are in acid form naturally. We use physics-based procedures to yeild an unadulterated product with as little temperature as possible to avoid any compound degradation. Yes you can have pure thca acids it’s all in the process. For example you may yeild 99% isolate but only have a return of say 20-40% whole oil weight in a week long procedure. Ex2 93% isolate potency but return of 55% whole oil weight in a day long process. From these two circumstances you can see if you alter time involved with isolation you can increase purity but it’s at a cost your return yeild from the process. Imo the impurities in the lower 90% thca make it more distinguished than pure isolate as it has trace terpenes and minor cannabinoids more or less giving you the best of both worlds high purity with slight characteristics of the strain it’s self

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can you further elaborate on this topic, perhaps a reference to some scientific data? Or some theory?
Do you mean in your biomass or in your butane?

To postulate the cannabinoic acids are in R- COOH requires some. Imagination. There is some academic work on THCA isolation R-COOH form, but the material is forced into that form with an HCL solution. That type of material is a white chalk.
Your product is very nice crystalline material.

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Yes all dabble concentrate pre decarb has coas to support this notion of thca being an acid form natural as referenced with the a ending in thca compound stated. I thought this was a publicly accepted fact that thca occures as an acid in the plant hence the thca in virtually all flower/oil? Yes they would stay in acidic form in solvent/oil matrix all the way from biomass back to finished oil/concentrate/isolate.

The batch your referencing was as we refer to as hot crash post extraction then was washed to get bigger isolate formations. Commercial thca methods typically are flash crash and are much finer in appearance simmilar to chalk as you brought up

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Yes, early on when “flash crash” was considered a problem I was one of the few people to advocate for using it as a feature.
You do understand that when doing RP HPLC chromatography
no matter what your crystalline form is, if you redissolve it in HPLC protic polar buffered to pH 2-5 you will only get the “form” of cannabinoic acid that predominates at that pH in that protic polar buffer. Capisce?
You don’t think that the peak you see on a RP HPLC chromatogram represents THCA in the R-COOH form?
Do you?
and that is your answer? What are butane extractors doing? Other than butane works and miraculously their “crystals” fall out of solution of thousands of unknowns and they sell it and make money.
Now I would say business-wise you know what you are doing.
I like your crystals
but somewhere there may be a CRC integral spool with an acidic medium in it for clean up???
Prolonged washes with water on recrystallization? I.e., LLE clean ups for the diamonds?
I am open to the idea that the bulk may being R-COOH in situ in the terpene phase of Capitate trichomes. In fact I wrote a little note about how this may occur just recently.
The problem is THCA is released from the synthase enzyme as the anion into the aqueous phase of the Capitate storage area. It is more of a question of how this anion gets protonated or otherwise complexed and partitions into a nonpolar aprotic terpene phase. The observation is , what ever form, it is clearly extracted into butane at -40 or so, and by some fiat later precipitates as a crystalline form. Nice. but RP-HPLC does not tell you what form that is , only the form that exists in the mobile phase buffer. That multiple forms exist can be demonstrated by looking at RP HPLC elution profiles of THC and THCA in various buffers in the pH range of 2.5 to 5.5 .

I still like your crystals.
If you can do a butane only extract, fast crash and get X-ray diffraction done on crystalline forms
I will be more convinced. (Yes exactly that has been done with CO2 extraction method that only extracts about 2% of the THCA and is acidified by the Carbonic acid that obtains
to yield the only THCA X-ray data). But there is not data on THCA purified that has not been exposed to Acid. Moreover, we do not know what is left in mother liquid. It would be interesting to know the mole ratio of “THCA”. left in the mother liquid.

Even more mysterious, is how and why does the “chalk” form precipitate out at the base of the extraction tube?

I think the “chalk’ form is THCA (R-COOH) , cannabinoic acid. If it is going to fall out in the extraction tube
why doesn’t the rest precipitate at this stage.

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What other forms of thca have you seen in coas of isolate or concentrates? We can look into getting xray done but lcms would be just as sufficient and easier to come by in standard cannabinoid test facilities, as our in-house analytics are unfortunately not running in same states where our manufacturing labs are.

We do know what’s in the mother liquor up to 80ish and 90% of oil composition has been identifed. Typically the hte fraction from isolate process are 35-50% thca any where from 1-6% thc based on farm and 30-40% terpenoid solution

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I don’t think you understand the point he’s making. THCA dissolved in water will be deprotonated as it’s a weak acid. It will also be deprotonated when dissolved in chromatography solutions – so whether it was protonated or deprotonated in the original plant, it’ll look the same on HPLC because it’s always going to have a certain ratio at whatever the pH of your mobile phase is. In fact this is why the broadness of THCA peaks on an HPLC will change quite a bit depending on the pH you use


The plant synthesizes the molecule as THC-COO- (deprotonated), because the enzymes that produce it are in water, and as an acid, the THCA is naturally deprotonated in water. So to say you extracted THC-COOH (protonated), requires the assumption that the original molecule, biosynthesized in water as a deprotonated salt, somehow gets protonated somewhere on it’s route to the trichome.

He is questioning if that actually does happen. Chromatography can’t distinguish the deprotonated salt and the protonated acid, as I explained before, because they will just transform into each other once in solution, and that will just depend on the pH of the chromatography mobile phase. For this reason one couldn’t prepare a “THC-COOH” and “THC-COO-” standard in solution for chromatography. One could, however, do so with solids, and run a test that can be run on solids, like the X-Ray he was suggesting.

But I think personally, that yes it is THC-COOH in the trichomes. I think it having been a salt would probably have been detected based on mass-balance considerations since the salt would have to have a counter-ion of different mass. And if the counter ion is metallic then even a test as simple as Atomic Absorption Spectroscopy could show that to be the case.

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No matter what form you have dissolving in RP-HPLC mobile phase buffer is going to “white wash” that sample.

There is only one study where the HPLC MS researchers wanted to avoid the possibility of “RP-HPLC” mobile phase and column effects on the same. You skip the HPLC analysis and do FIA (flow injunction analysis “ directly into the ion spray port of the mass spec.
Using Cerriliant standard THCA this is what you get


High Resolution Accurate Mass (HRAM) FIA Experiments
A quadrupole time-of-flight (QTOF) mass spectrometer (Agilent Technologies) equipped with a dual ESI source was used. The QTOF was operated in ESI+ mode over the mass range of 100–500 m/z . Samples were directly infused into the electrospray source with a syringe pump at a rate of 200 ”L/h.
P.J.W. Stone, S. D’Antonio, N.C. Lau, W.A. Hale, and A. Macherone, Cannabis Science and Technology 3 (3), 34–40 (2020).

Unless you are doing FIA
you are only looking at mobile phase controlled properties of cannabinoic acid “forms”.
However, the elution of cannabinoic acids vs pH of mobile phase tell you a lot about physiochemical properties in the pH range 2.5 to 4.5.
Sambo Creeks ionic charge separator of trichome heads produces an excellent material to do the ICP-AES
analysis of that restricted volume element
.we should know that number soon especially the K+ and Ca++. Knowing the upper limit of THCA concentration in the trichome head fraction is very helpful. If you had a tightly bound complex of say K+ with the anion fraction that may exist
HPLC would mask it. Remember, it does not have to be one form or the other, it is a mixture ! Exactly what the chromatogram peaks represent unless you force them to pH 2 or pH 5 with selective buffer. Delta elution order per delta pH change is instructing you the mixture ratio is changing. But no matter what intermediate mixture you have you only see one peak.

Nice crystals and “butane works”.
@Octave, only about 1 in 20 Ph.D. Chemists have studied Studied “Separation Science” as a formal graduate level topic. If you had, a quick look at any RP-HPLC chromatogram of Cannabinoids would immediate alert you to the fact that something odd is going on. It depends on pH mobile phase buffer, but in general you will see CBDA/CBD elution order is reverse that of THC/THCA elution order. ( Like a standard C18 column and using a water methanol/ formic or acetic buffer as Mobile phase.)
So what ever is going on with THCA is not happening with CBDA. So the question is: what is the “form” trapped in the Nonpolar C!8 column support, R-COOH proper, or an Intramolecular H-bonded Anion form, once formed can partition into non polar
by itself or in association with the neutral form (acid homologous base pair). The Decarb- kinetic studies of H. Perrotin-Brunel et al. / Journal of Molecular Structure 987 (2011) 67–73
strongly suggest that some small acid or water is trapped in THCA isolates.
There is some odd behavior exhibited by purified THCA that is not completely explained.

Octave, your crystals and lab work to produce them, looks as good as one can expect in the industry. So hopefully this extended discussion brings some attention to your product and stimulates further studies about the detailed chemistry of THCA both anionic and neutral forms.

When you look at someone doing HPLC ESI MS or one of the many hybrid forms of MS, look closely at the choice of mobile phase of the HPLC.

Addendum edit:
Here is an example of someone who clearly understands the “mobile phase white wash “ problem:

“The isocratic LC conditions were developed to separate the target analytes from the family of congeners likely to be present in C. sativa extracts, and to generate the best peak shape. Formic acid was used to buffer the HPLC mobile phase to generate a single conjugate of the acids during chromatographic separation.”
A reliable and validated LC-MS/MS method for the simultaneous quantification of 4 cannabinoids in 40 consumer products

“ using an isocratic mobile phase of water (0.1% formic acid): acetonitrile (0.1% formic acid) 10:9”

Here we have a case where 0.1 % formic and the pKa alteration of the 90% ACN b phase
.probably achieves a high ratio of R-COOH/R-COO-. Interestingly, when you do ESI of standard THCA you get the 357-H, and you simply do not know whether your are doing a gas phase ionization of the carboxyl with remote loss of H or the H loss is anion.??? the dynamics of the ESI process when you get down to it, are rather mysterious when it comes to R-COOH vs R-COO- as conjugates. Someone needs to do direct FIA of THCA and CBDA in a suitable buffer, pH 5 MeOH/H20 90/10 and MSMS, negative mode. N2 gas.

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Nice glad we’re generating discussion well look into the isolates properties relating to protanation

Thanks for the positive feedback and respect

It’s amazing that we get to do this, it’s dope we all get to work together as a community we continue to move them in the right direction

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What about the interim final rule or final rules which calls for POST decarb testing?

You can’t choose which rules to follow and which ones to not

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Look
we ALL want to know


How fragile is this? Can I wire wrap it? Do they fall apart when shocked?

Just wondering, cool stuff @Octave!

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I see

Proper crash does hold its structure quite well but is still typically fragile if facets aren’t flawless. As each imperfection yeilds stress points along the microfractures resulting in a less hardy formation. Short answer is yes if you have inspected it and do a quick pressure test at various points

With the right care and skill, the crystals could be wire wrapped with a high purity, gold, potentially adorned with different colored diamonds, depending on natural Fido chemicals stain present from terpenoid patina
Comparing THCA crystals to something else in structure, they might be likened to hard candy or rock sugar in terms of hardness and durability. Like hard candy, they can resist some pressure and handling but will break or shatter if enough force is applied. The comparison isn’t perfect, given the different chemical compositions, but it gives a rough idea of the physical properties of THCA crystals
Your inquiry does inspire me to develop someThca jewel pops

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Screenshot_20240302_111314_Gallery
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@blow

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THC a tub! Let’s see the diamonds!

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Talk about a picture that speaks a thousand words.

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This is solid. I have a few inquiries for 10 kg a week small/med :gem: . If this pricing is right we can play ball :). DM’d you.

I have what can be called ‘frosty diamonds’ for an extremely good price as well, but I’m not trying to hijack your thread. We can talk if you wanna distro these.

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