Wednesday, December 05, 2007

Compound Characterisation in Industry

As I have mentioned previously I'm back working in industry/biotech. One of my colleagues asked me an interesting question today:
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What is the golden standard for compound characterisation in industry?
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Where we work now we only do 1H NMR and LCMS. However, in my previous industry job we also did 13C NMR, full on 2D NMR and elemental analysis. What are you industry people out there doing and what are your views on this issue? D!

8 comments:

HB said...

Melting points of the unknown's tosyl hydrazone

Ψ*Ψ said...

Doesn't it depend on what it is you're making?
I'm not working in industry, but in my current (academic) group...if you've made something new and exciting, but don't have a crystal structure, you face a little skepticism.

milkshake said...

If I just put a sidechain by amide coupling, I take TLCs as it comes off the column and HPLC of the combined purified stuff, to make sure the compound is really pure and LCMS to see taht it is the right compound. I don't bother with NMR. When the time comes to write up a patent application procedures, we have to take NMRs of all final compounds (NMRs of all intermediates are good to have but not required).

I take NMRs (besides LCMS, HPLC) on all intermediates whenever there is question about purity, salt forms, isomers. But most of the time the chemistry of kinase inhibitors is very simple.

Daniel Sejer said...

Milkshake, wouldn't you say that 1H NMR is adequat for patent purposes. I'd certainly hope so since we are not doing 13C NMRs at this stage. D!

milkshake said...

Nah, for patent purpose you just need to prove that you made your compound in the experimental example, that you did not "prophetise" it up. I am always very sceptical about patents that have only a MS as a characterisation: M+1 mass is not that hard to fake.

The standards for patent submissions are much lower than for publications. All that patent referee does is checking the claims - if the compounds are new, if the claims are supported by the examples and so on.

Daniel Sejer said...

How about publication in scientific journals? If all your getting is 1H NMR and Low Res MS you can only really publish communications and letters. In my first industry job the boss/company was very determined to publish everything in journals the second the patent was out. Hence, we where getting all the necessary analytical data etc. for this. The only catch was that we had to write papers in our spare time (i.e. at home). I think that was a fair deal since it looks pretty good on the CV and improves your career prospects. D!

milkshake said...

I did not publish much, on my medchem work, what I wrote up was usually on methodology, and usually done as a side-project. It depends on the company. The startups usually publish a lot (sometimes even more than they should) to impress the investors. Once it becomes a large corporation the process is more bureaucratic, you need to go to great lenght to convince the superiors that the stuff should be published and so on. Again, companies differ.

Also, J.Med. Chem. (or even Bioorg. Med. Chem. Lett. or some godafull biology hournal) have much lower standards than say, JOC.
So may get away with just 1-H, and LC/MS. Not that it should be a norm...

Daniel Sejer said...

Milkshake, J. Med. Chem. used to have very high requirements for analytical data - higher than JOC. However, with the recent changes to the JOC requirements they may be as strict as J. Med. Chem. now. Anyway, as you suggest, one can always just go for letters and communications as these generally don't require any analytical data at all. D!