Aqueous Wash Of BDTs

For one reason or another, we once tested washing some botanically derived terpenes with water as a step in an unrelated process.

Mixing with a fair amount of water, heavily agitating for a bit, allowing phase separation to occur, than capturing and carefully drying the terpene layer.
Changes to smell of solution had been immediate and pronounced, in an interesting way. Overall the intensity/stregnth of the odor was significantly diminished,
some of the heaviest notes seemed to be lost altogether, and other subtle components of the fragrence that did not seem to express well before were now more apparent.
Essentially they got lighter overall, and the more subtle notes that were being overpowered surfaced.
It seemed to pull away a bit of that chemically smell that terps sometimes get as well. Initially, this didn’t make much sense to us.

Yes, terpenes in the presence of water + heat (steam) and/or other substances seem to undergo some mild decomposition reactions and alterations.
However, the initial test was performed without the presence of any heat. In addition to this, we assumed most of the oils present would only be sparingly soluble if that.
We were fairly certain it was unrelated to a change in concentrations of major components (say the aqueous phase was pulling slightly more of x then y).
That lead to the idea that perhaps a minor impurity of a terpene isolate, or an oxidation product of the mixture was responsible.
Very small amounts of impuritys or oxidants can have a staggering effect on the overall smell, taste, and sensitivity index of a complex mixture or single compound.
What they were, and how they were migrating to aqueous phase was eluding us (specifically in the case of what we had suspected to be things like hyperperoxides, plain terpene isomners from degradation, ect).
We figured things like acids, solids, epoxides maybe, ect could feasibly be migrating to the aqueous phase. Anyways, we decided to make testers from the recaptured terp fraction.
Taste wise, the results very similar to almost identical effects overall to what it imparted on the smell. The overall intensity was reduced, the heavier notes seemed to be hollowed out, and the subtleties surfaced.

The interesting part was a noticeable lack of irritation or heaviness that is normally associated with BDTs.
They were certainly much less “harsh” at equal concentrations than the source terps, or any of our BDT preparations in general for that matter.
The initial test was repeated on a variety of terpene feadstock with varying concentrations of various terps, as well as single compound terpene isolates.
We generally saw the same trends (lack of irritation, reduced intensity, lighter notes becoming more prominent/pungent).
Some worked better than others, flavors got muddy in some cases, or even entirely changed taste/smell rather than mellowing out in very rare cases.

Now, we are fairly certain this is at least in part a result of things like acids (and perhaps ph change), solids, ect migrating to the aqueous phase.
However, i recently stumbled upon some literature “Stability of Essential Oils: A Review - Claudia Turek and Florian C. Stintzing” that suggests
hyperperoxides or oxidation products (additional hydrocarbons) could become more soluble in water once degraded, and perhaps partially move into the aqueous phase as well.

“A new approach combining conductivity and pH assessments has been applied to monitor storageinduced oxidation processes in essential oils complementing POV.
For that purpose, stored oils were extracted with water followed by
analysis of the aqueous phases (Turek and Stintzing 2011b). While
mere terpenic hydrocarbons are not soluble in water, oxygenated
derivatives were shown to partly pass into the water phase upon distillation, most likely owed to the capacity to form hydrogen bonds
(Rajeswara Rao and others 2002; Edris 2009). Moreover, Borglin
and others (1950) as well as Mercier and others (2009) reported
that terpenes became water-soluble upon oxidation. Chapard and
others (1972) observed the same effect in oxidized essential oils.
Less stable hydroperoxides and epoxides, formed as intermediates, were suggested to be hydrolyzed into terpenic polyols in the
presence of water (Borglin and others 1950; Lorand and Reese
1950). As a consequence, polar, conductive, and/or acidic secondary products accumulated during terpenoid degradation and
subsequently passing into the water phase, might be captured by
combined conductivity and pH measurements.”

This got me thinking that perhaps, in addition to things like acids, solids, maybe epoxides, ect we could potentially have hyperperoxides and terpene degradation products in the aqueous phase.
Certain hyperperoxides leaching into the water could also feasibly explain the marked difference in irritation, and in some cases smell/taste.
Hyperperoxides and oxidation products can in many cases work as signifigantly greater sensitizers or irritants than the parent compound they spawned from.
They can also exhibit significantly different taste/smell from the parent compound, potentially at significantly greater intensity.

With this in mind, we are experimenting with washing our entire index of strain mixes in this way, and are seeing very positive results in most cases (~90+% of source terp samples seem to go well).
In regards to things like hyperperoxides and oxidation products, all terpenes on our end are stored under ideal conditions after they are received from the manufacturer.
The feadstock terps we are using aren’t old, nor do they seemingly have much general oxidation overall.
We have tried using different vendors terpene isolate stock as well, and well there is some difference in what happens via a wash vendor to vendor even with the “same” source isolate, the trend continues.

We are working on securing analytics capable of testing the aqueous phase as well as the end product terpenes vs the source bottle, but we aren’t there yet.

So, i will propose the question, what do you suspect is going on here? What compounds or types of compounds, exactly, are migrating into the aqueous phase?
The marked lack of noticeable irritation or harshness has us utterly intrigued because generally, that’s one of the main complaints in relation to botanicals.

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@stoopkid might have some insight

You are essentially partitioning the terpenes between two phases, in chemistry this is known as logP the octantal water partioning coefficient. Octanol-water partition coefficient - Wikipedia
If you’re curious you can look up individual compounds value to see which fraction they might end up in.

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Why guess and wave your hands?

If you’ve got naught but organoleptics, find a third party lab to tell you the difference between A & B.

Do it with almost freezing water(4c) let the layers seperate then freeze the whole solution at -10C. Pour out the terps.
R u talking about cannabis/hemp derived or botanical as in from other plants/fruits/etc?

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Yes. It is possible you lost some terps to the aqueous phase. You could check that out by putting a few drops of the water after washing into pure methanol and running it on terpene gas chromatography analysis.

We don’t plan on utilizing anything in production until we can get some samples ran, obviously.
Isolates and in house strain mixes from them are cheap enough so as the cost of a couple of ml to test procedures is totally negligible in the scheme of things.
However, getting panels ran on even one of those is going to cost way more than all of the source materials used, something like 10 fold.

The end goal is to get panels ran on everything and get a solid grip on what’s occurring, but we cannot justify the cost it would take to test every strain mix (quite a few) twice as you describe at this time, in addition to testing all of the single compound isolates. We also have the concern of the exact concentrations changing as they age (post processing in water), new oxidants, ect being formed over time. So potentially a third test per vessel…
In addition, we are always tweaking, alternating, ect on end mixes, as well as sourcing isolates from new suppliers. The amount of analytics required in the grand scheme of things would not be trivial.
We do intend to get a test sample ran soon, however we are thinking a variety of compounds are getting pulled depending on the exact mixture or contents of the individual isolates in the mixture so im not sure just how much insight a few tests will actually offer.

Generally, we are trying to get some idea of what types compounds would be pulled, from a variety of different isolates and mixes. The next concern for us would be how those ended up in the specific mix to begin with, what concentrations they are present at, potential implications of having those in the mixture, ect.

At this point, this is mainly pure R work, and we are trying to potentially reduce overall costs and gain some insights without going crazy on investment at this stage, to see if this is even worth majorly exploring (and absorbing the large costs associated with testing hundreds of samples.).
Appreciate all the insights so far nevertheless!

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Generally just botanicals. We did try it on some hemp terp as well but the results didn’t seem to be nearly as profound in any regard.

In regards to freezing, i would imagine separation would be more convenient as you describe assuming you wanted to wait for it to freeze but i wonder what type of effects on absorption of certain compounds into the water phase, or overall chemistry, reduced temperatures would have.

I have seen rapid temperature changes result in odd effects on terps before so im unsure, but i may give it a try just to see, thanks!

Short answer: this is a bit of a loaded question that I can’t really answer without analytics. Too many unknowns.

All terpenes are going to contain non-terpene compounds. Highly refined isolates still will often contain traces of aldehydes, terpene oxides, epoxides, unknowns and more often than not a mix of other terpenes that came along for the ride. A blend of isolates at varying purity levels would be more unpredictable in this sense. Some compounds can definitely be lost to water (partially or entirely, like silverstudent explained), others can produce byproducts when exposed to water/air.

For cannabis terpenes, this process pretty much already would have taken place before you got them from using salts/sep funnels so I wouldn’t expect a major change. I really can only guess what an “after” might look like if I had analytics for the “before” in front of me. I mean I could find out if OP really wants to test a before and after sample of something. It’d take a couple weeks. I wouldn’t be able to find out what’s in the water portion.

You’d be better off just pulling a sample of the terps before washing and running it again after. There’s really just a lot of variables at play. Some things will be lost to the water, some things may react with it and produce new things. Then some new compounds could simply have just been below the detectable threshold before purifying them and show up after. You’d just have to do a side-by-side comparison of the results. Too many possibilities to make a realistic guess here. One of those times that the only real acceptable answer is “labs.”

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