USP Residual solvents chapter <467>

[amarla]

Has anyone been able to successfully analyse USP <467> on an Agilent 6890 GC/headspace, using the method as it is written in the current issue (USP 30)? I am using a Restek 624, 0.32mm, 1.8um, 30m, Helium, split ratio 5:1. I am finding it hard to identify the Class 2 Std A and Std B peaks (without doing a heap of upfront work, or injecting the solvents individually!) I have tried the test for water soluble articles, procedure A, using the operating parameters suggested in the table (conditions 1 and 2).
Many thanks!

[Schmitty]

Without using an MS, I don't know how you might identify the compounds without injecting individually.

I am runnig these by GC/MS and am only having issues with pyridine and nitromethane.

I'd give you the elution order on my column, but I fear that my employer may flay me

[Alchemist5]

Maybe this may help

http://www.restek.com/aoi_pharm_A013.asp

[Schmitty]

Nice application note, thanks. Notice the peak shape of the pyridine and the sensitivity of the 1,2-dimethoxyethane