Anyone ever run a method of reverse phase that effectively isolated D9-THC?
I have hundreds of hrs of flash and preprative chroma work under my belt, but never was asked to isolate D9…
Anyone do it yet?
All I can find on literature is the Dronabinol patent using a totally different technique of approach.
Im starting to think I cannot seperate D9 using C18 solely.
Not C18
https://pubs.acs.org/doi/10.1021/acs.analchem.0c04592
Although using protein rather than dna would allow easier scaling.
What about this paper, that looks to have some level of D9 separation? It looks like it’s a C18 based stationary phase.
Preparative_THC_Purification.pdf (308.7 KB)
Sure, the peaks aren’t completely clean and the cis-d9 peak looks to be very close to eluting at the tail of CBN, but I’m sure there can be some further optimizations. I haven’t tried this yet, and it’s obviously a publication by the company selling the stationary phase, so there is always the possibility of some kind of data manipulation in favor of good separation, but it’s a starting point.
I guess it would also depend on how clean your sample is before you try to isolate it and what other cannabinoids are present. Or go with a CPC and isolate with a CPC instead of traditional chromatographic methods such as flash or preparative chromatography.
RP HPLC does not have the capacity . Period. It is not that there are not 1/2 million dollar systems that could do it…you can not afford the high purity solvent to do the separation at large scale…vs what your THC is worth. Moreover, ultra high purity THC is not exactly a commercial product in demand., A little bit over the top in strength and no taste.
Crystallize THCA….decarb it and go…you are not going to get more bang for your buck….even less expensive…just dab the THCA…
Yay aptamers in the wild. I used to play an online game with the user name aptamer.
Someone was claiming that molecular imprinted resin was the future of isolation a year or two ago for isolation.
Yeah, the people making bank of hplc are selling nano and micromol of substance for tens or thousands of dollars per few mL.
Interesting , the nanomolar affinity “Ka” certainly is an attractive feature: selectivity factor. This is the first I have heard of screening large libraries for “aptamers”. …but seem functionally equivalent to resin bound monoclonal , affinity columns.
It would seem the industry has made judicial use of “dirt” so far as commercially marketable products are concerned.
fine chemicals is not this industry.
I will sell you a 25K chiral column for 12K if you want to do it right.
What’s the reason you wish so pure thc ?
Melt recrystelize thc-a and take to 90 C while argon sparging treu solution and keeping an argon pressure on the vessel of 15 psi and a prv venting at 15 psi all the time you ll need MS to get a decent reading hplc can t
Some dimers of thc will be formed but less then 0.3%
@Roguelab
I’m curious about the thc dimers. Can you explain the form?
“take to 90 C while argon sparging treu solution and keeping an argon pressure on the vessel of 15 psi and a prv venting at 15 “
Have you been hanging out at the university? that is a bit of a “twist”…nice. What about adding a few drops of water for a catalyst?
Yes a theory we are starting to suspect is that when decarboxilation occurs
Dimers are created and andthey fall appart ideally but a minor amount does not don t know much as to how the theory was tested by the university
And pretty intensive do not really know what they did to get to the conclusion
As you know I am diving in the isolation of cannabinoids to pharma grade
Cbd-a a
Redacted
Op is asking for purification of thc D9 that doesn t crystelize so not an option
That was meant to be a response to you though… no worries - removed!
pharma grade in a lot of contexts means total synthesis because they straight up don’t want it plant derived. not always the case, but definitely common.
I have some contacts in the pharma world…
They say 98% or better can be refined to API standards and be used/sold within the pharmaceutical industry.
sure, in some instance. Both ways are not uncommon. In others instances, the company may specify total synthesis. Its not solely about hitting some threshold purity number - they need to consider impurity profile, raw material specs on incoming materials, inherent variability the comes along with plant derived products, vendor reliability, so on/forth.
Consider that if you’re able to sell a product for whatever price you want and you have all necessary vendors in place that can hit your raw material specs for total synthesis then there is little motivation to confront the complications that come along with a plant derived starting material. One company might be cool with plant derived raw materials, another company might insist otherwise.