I’m looking for methods of detecting fake T-free distillate, ie cut isolate versus reverse phase chromatography (apologies to new techs that might be out there). So far, I deduce…
(1) CoA should have CBG present. CBN may be present, but likely with the THC fraction (along with CBC).
(2) Dissolve in cold methanol. If it won’t dissolve, lots of non-polar compounds may be present that shouldn’t be present, indicating possible cutting agent.
Am I off-base? Are there any other “tests” to apply? I’m seeing T-Free distillate north of 95% for sale… and I can’t help being suspicious.
Thanks Rowan. That is my preference. Unfortunately, their are a lot of suspicious people in the industry that won’t do show and tell, let alone sit in during processing. Part of me doesn’t blame them… the upcoming patent carnage will be ugly, with accusations and counter-accusations of infringement… even though 90% of published patents are going to get tossed due to prior art or obvious…
you could run GC for solvents and see if there’s any residuals in there indicative of chromatography or processing. I’m not sure where you got the idea that presence of CBG or CBN necessarily indicate “legitimacy.” Its almost certainly a prudent question to ask what your definition of legitimate T-Free distillate is because there are any numbers to reach a THC free product including but not limited to chromatography. For instance, if the definition is a mixture of > 95% cannabinoids with non detectable THC then I dont really see how CBG or CBN necessarily fit that narrative. Certainly, if you’ve got like 80% cannabinoids and of that its 100% CBD and no other cannabinoids you’ve got a red flag. As an aside, god help anyone unimaginative enough to spend their days running RP chromatography on scale recovering drums of solvent (or god help them if they’re recovering water) and blowing their load on RP silica just to run a few kilos.
We produce “T Free” (<.04%) distillate using c18 columns and consistently get 95-97% cbd 1.5-2%cbg and .5-1% cbdv.
Higher purity doesnt mean its been diluted with isolate. My opinion and experience would be if there is little to no CBDV then its likely being diluted with isolate. But you also have to keep in mind the levels of minors is strain dependent.
We use a simple glass column with c18 and manual fraction collecting and in house analytics for testing each fraction. (agilent 1100 HPLC)
We do a 3 step gradient which absolutely blows when it comes to dealing with the separate solvent blends but it does give us great results and good separation from thc.
We also are not starting from distillate, this is from hexane extracted, winterized crude that has been ran through a few other columns to remove impurities. Before it goes into chromatography were at 80-90% cbd. Then it comes out at 95-97% cbd.
This is also not going through a short path or a wiped film.
That’s 800g of CBD if you have 3% CBD loss then (800 - (800 x 0.03)) = 776g of CBD in your final product or 24 grams of CBD loss
Let’s assume the same 3% loss for CBG and CBDV
CBG: 1000 x 0.02 = 20g of CBG to start with
(20 - (20 x 0.03)) = 19.4g of CBG recovered or a 0.6g loss
CBDV: 1000 x 0.01 = 10g of CBDV to start
(10 - (10 x 0.03)) = 9.7g of CBDV recovered or a 0.3g loss
Then for CBC and THC we have
THC: 1000g x 0.03 = 30g of THC to start
CBC: 1000g x 0.03 = 30g of CBC to start
Let’s say we totally remove them… so 60g of loss
Now let’s say we also remove other impurities via Chromatography and so our total cannabinoid number increases from 89% to 95%… indicating a 6% loss in mass from impurities
1000g x 0.06 = 60g of impurities lost during purification
So if we have 776g of CBD in our final product and it weighs 855.1g then it’s 90.75% CBD in your final product. CBG is elevated to 2.27% and CBDV is elevated to 1.13%…
So it is possible to get 95% CBD T-free from something that is say 85% CBD and 90% total cannabinoids…
Not trying to rant on anyone, just sharing knowledge
I’m curious if its this hard to distinguish chemically true T-Free made by column vs cut with isolate then is there actually a difference we should care about in effect?
Isolate is going to be stripped of all other plant material while distillate is going to have other plant material still in it. Essentially whatever your total cannabinoid level is (ie 96%) you will have 4% of unknown plant material.
Also isolate diluted distillate will not have as low levels of THC compared to a properly ran c18 column. The labs doing this are most likely using a 3rd party lab with higher LOQ and they are doing simple math to figure out how much isolate they need to dilute the distillate with to get below their labs subpar LOQ levels.
Ahhhh ok. Damn that sounds like it takes foreverrrrr. What’s the output speed after it’s gone through columns like 5 different times including filtration and all that
For whatever reason it’s very typical to see weight loss and potency loss. Which to me makes zero sense.
And there goes @RockSteady chiming in once again. Never stepped foot into a lab, but my mans down to try to put his 2 cents in everywhere he goes. Why you here again?
I think someone’s a little salty they cannot run chroma properly; just the other day you posted a thread about running c18 without gradients; and now your an expert on the efficiency of c18 separation because you flowed some solvent through a column?
Salty boys going to be salty.
Oh and just btw; if you cannot get perfect separation via c18; analytical chromatography would not work the way it does. Rekt.
Um… what do you mean? This is one pass through the column…
Load the cannabinoid solution into the column, then you load your 3 gradients into the column one at a time. Each gradient allows the compounds to separate further. We would not have the purity levels and low levels of thc if we did not use a gradient.
Not running a gradient on c18 is a massive waste of time and money.
As @RockSteady said this is exactly how an hplc works, it has a built in gradient pump that makes your gradients for you and causes the peak in your graph to actually separate.
We use this exact same concept and increase the size of the column and do these automated steps manually. Voila separated cannabinoids!
