Standard Operating Procedures

This Standard Operating Procedure (SOP) describes basic chemical safety information for Mass Spectrometry (MS). Prior to conducting work with a mass spectrometer, personnel must obtain approval from their Principal Investigator (PI) and/or Supervisor and attend the appropriate mass spectrometer usage and sample preparation procedures.

Additional Information

Basic operating procedure:

Book a slot for the mass spectrometer at LB009

  1. The system should be switched on. If not contact the lab manager.
  2. Load your method.
  3. Allow the instrument to warm up.
  4. Prepare the sample in a fume hood, biosafety cabinet, or glovebox and not in the ms room.
  5. Ensure that the system is behaving normally and that the temperature and pressure are stable.
  6. Load your samples in the auto sampler and setup a batch analyses file. Don’t forget to include a standby method at the end.
  7. Once your sample run is complete, allow the instrument to go through its cleaning cycle.
  8. Remove all sample vials.
Sample preparation

The following approach is recommended for making up samples for the High-Resolution mass spec analyses:

All samples need to be filtered. Dissolve the sample in organic solvent (e.g., DCM, CHCl3, EtOAc, MeCN, MeOH) or H2O to a concentration of 1mg/mL. Please do not use low vapour pressure solvents, such as DMSO, or dilute them >20-fold in another solvent.

Take 10µl of this solution and dilute it with 1mL of either methanol, acetonitrile or water (or any combination of these solvents).

If there is any precipitate in the resulting solution it must be filtered before running the sample otherwise this is very likely to cause line blockages and delays with sample analysis for all users.

Place the solution in a standard 2mL sample Mass Spec vial with a screw cap lid and soft split septum on the top.

Do not use Trifluoroacetic acid (TFA) in your samples. If you need to acidify your samples use formic acid.

Do not use Tetrabutyl ammonium (TBA) in your samples (also avoid other ion-pairing agents) these will contaminate all subsequent samples run on the system.