No headspace autosampler

[Dominique]

Hi everyone,
Has anyone tried to adapt the residual solvents method in USP- 467 to use a liquid autosampler? If it could be done, would it require full validation? What injection parameters would you recommend?
Thanks!

[Ron]

USP <467> allows liquid injection or headspace for sample introduction, so many people have used an autosampler for this method. Start with autosampler defaults and a 1 uL injection, and change parameters if the defaults don't work.

[krickos]

Hi

If doing liquid injection you may need to keep an eye on injection temperature even before you start depending on what sample solvent (water,DMF etc) and boiling points of residual solvents you do analyse. If memory serves typical default injection temperture is like 140°C that may be too low.
Split ratio may also be tweak to optimise sensitivity.

If using water as sample solvent you likely need to reduce injection volume immediately to like 0,5µl for a ~1ml liner.