Anyone else have an HPLC method that gives good resolution between D8 and D9.?

You would think, but with all the new analytics operators in the field, nothing goes without saying. After all, people have spent a shitload more on equipment they have no idea how to run

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Anybody got any suggestions for applying this to prep/flash scale?

Do you use a prepared 10M solution or do you dilute the salts?

I find dissolving the solid ammonium formate in water and sonicating at room temperature for like 15-20 min gives the best chromatography.

You should be able to do both but I’ve noticed the prepared solution adds a bit of uncertainty that can alter the composition of the mobile phase enough to yield minor peak distortion.

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Yes, I read about this method… forgive the ignorance… how do you get a 10M solution out of powder?

10 x volume (L) of solution needed x molecular weight of powder = grams of powder to dissolve in amount of solution needed

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I can help you. I know of at least two methods that will give you baseline resolution of d8 and d9.

I also know of a second method that will yield a lone d8 peak with no other peaks close to it. Ideal for high concentration d8 samples

*peak #8 is delta-8

DM me for more info

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So forgive me what would that mean for ammonium formate in 1L of HPLC grade water or ACN?

plug this into the formula

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Hi IonStorm,

Hope you are doing well. I’m interested in the 2 methods that you mentioned that give increased separation of d8/d9 THC as well as isolating d8 THC from other compounds. Would you be able to provide the methods?

Would you be willing to share your method for baseline resolution of d8 / d9?

@ShuckleBerryFinn

Doing this at scale vs on an hplc are completely different endeavors. 75:25 MeOH:H2O with 0.1% FA with specific columns and flow rates will yield baseline separation/the 2 compounds having a RT almost 1min separate from each other. At scale, you have to use acidified gradients, and it is an exceptionally slow and solvent consuming process. The best I was able to achieve over about 2 months of experimentation was increasing the D8:D9 ratio from 80:10 to 96:1 in my fractions of interest (interchim 5.105).

There are abundantly easier ways to remediate D8 THC than flash chromatography.

I’m selling a thermo ultimate 3000 so I’ll plug that here as well in case anyone on this thread has a need

Hi IonStorm,

Would you be able to share your method?

https://www.preprints.org/manuscript/202403.0367/v1/download