Hi everyone,

I've developed a LCMSMS method for the detection of hexamethylene triperoxide diamine which has been running fine for the last 3 years. About 6 months ago I started seeing signal suppression which has only got worse. I've sourced my problem back to the solvent used in the extracts. (Acetone)

I've run the acetone on my GCMS (EI) and identified that diacetone alcohol has formed in my solvent. I've retried the whole process with a new batch with no problems.

Has anyone else seen diacetone alcohol causing signal suppression in LCMSMS (APCI)?


Method:
LC
Column: Alltech Alltima C18
Eluent: (Gradient) Start: 1%MeOH / 99% water; 1-10 min increase to 100% MeOH
Flow 0.2mL/min

MS (APCI) positive mode
Vap temp: 200C
Cap Temp: 220C