Failing Sulphated Ash Test on CBD Isolate

I did notice the same peak in the old distillate (that was run way too hot) so I dont think it could be CBDB?

Do you know what inorganic impurities would show up on a chromatogram?

According to this paper, this should be CBDB.

https://www.sciencedirect.com/science/article/pii/S2352340919308182

I never checked this with a standard, so far. I did not paid attention it is now available.
But I analyzed numerous natural cbd iso by GC, they often contain 0.1-0.4% CBDV, and always have similar proportions of an impurity coming halfway between CBDV and CBD.

Synthetic CBD is a rare product, I’ve ever seen one sample.

The mystery peak in my original post comes after CBD. So based on your info and that paper it likely is not CBDB since that comes before CBD, and between CBDV and CBDB

Indeed. :man_facepalming:
It should show up before cbd with hplc as well.
Still you should check closer, cbdv and cbdb should be there as well. Their contents can be decreased, but still persist after multiple recrystalization.

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I will ask them to check tomorrow.

Our CRMs from Restek are sketchy. The CBD CRM was recalled (they didnt even notify us till we reached out), and were seeing a bunch of minor peaks in their CBN, D8 and D9 Peaks. Same story actually with the CBDV CRM from Emerald Scientific. Im not well versed enough in this to know WTF is going on. Major pain in the ass for pharmaceutical validation work.

The mystery peak was also in the distillate, so it couldnt have come from the hexane.

Mystery peak coupled with failing inorganic sulphated ash test still leads me to believe its a heavy metal? But so far we havent detected any with 3rd party lab. I will send for more testing tomorrow

I take it your in Switzerland. Grüezi.

This is an HPLC chromatogram from lipomed in Switzerland. Are those 2 bumps in the beginning CBDV and CBDB you think?

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Yes. :switzerland:

I believe cbdv and cbdb would come closer to cbd.

What is the actual DL on these hplc test of these cbd isolates ? And what are the cbd contents measured ?

Also did you envision that the inorganic impurity detected by ATG and the one in the hplc chromatogram could be different ? Were replicate analyses done ? Do you have a ref material passing sulfated hash test with success ? :thinking:

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How much for the @Dr_Jebril and @Roguelab European tour where you get a view of all angles of the euro industry. :heart::heart::heart::heart:

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Now that I remember.
I have sometimes tested isolates wich had another notable (and detectable) unkown, showing after cbd and before d9-thc. These where in general yellowish isolates, where the chromatographic purity (detected components) is high, in the 99%, but the quantitative analysis is rather in the 97%, hence with more undetectable impurities (likely waxes).
These products also generally leave a dark or redish color on filters, when important quantities are filtered in solution…

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This is the CBD in question

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3 samples

Quantatative:

A:
CBD 100.3%
Mystery Peak 0.1547%

B:
CBD 99.39%
Mystery Peak 0.1562%

C:
CBD 99.45%
Mystery Peak ND

Sulphated ash test were doing with a reference material today and waiting for the results from a third party lab which has a muffle furnace to make sure were not causing inaccurate results since we were using a burner.

Also doing a methanol test to check for fats and waxes.

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Problem was solved. Tested at independent labs and got 0.038% sulphated ash where monograph dictates <0.1%

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That’s a relief :sweat_smile:

Good news that the analysis showed less 0.1%.

Did you ever test for CBDB?

Seems like you guys need to beef up a few things in the QC/QA department to avoid such issues in the future…

One thing that comes to mind is QC/QA inspection, testing and release of incoming raw materials (i.e. solvents, etc) and another is analytical method validation, including QC/QA of CRMs.

You can get away with skipping this in the US but to adhere to EU GMPs it’ll be a must

Just my 0.02

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100%. Have to be incredibly thorough. No short cuts. I think it was a combination of the silica crucible and using a burner rather than a muffle furnace. No real way to control the temperature with a burner and the sulphated ash test calls for 600 Celsius ± 50 Celsius. Obviously burner not ideal.