Phthalate analysis by gas chromatography–mass spectrometry: Blank problems related to the syringe needle

For the analysis of the most commonly encountered phthalates by gas chromatography–mass spectrometry (GC–MS), absorption of phthalates from the laboratory air on the outer wall of the syringe needle is shown to be an important contribution to the blank problems. It was investigated for programmed temperature vapourizing (PTV) injection. Cleaning of the needle in automated injection is of modest efficiency, since the needle cannot be immersed deeply enough into the wash vial. Two approaches were studied to minimize the transfer into the column: (i) cleaning of the needle in the injector prior to splitless injection by inserting the needle in split mode while the precolumn is backflushed, which presupposes a high injector temperature to be efficient; (ii) injection under conditions minimizing thermal desorption from the needle wall, i.e. fast injection at low injector temperature (e.g. 40 °C). Both approaches resulted in blank levels of around 0.1 pg for diisobutyl phthalate (DIBP) and dibutyl phthalate (DBP), and of around 1 pg for di(2-ethylhexyl) phthalate (DEHP). They could be useful tools in existing or future methods for the analysis of phthalates or other compounds causing blank problems through contamination of the laboratory air.

► Outer syringe needle wall was found an important phthalate contamination source.
► We tested approaches to minimize phthalate transfer from the needle into the column.
► Cleaning by solvent in the wash vial of the automated system is poorly efficient.
► Cleaning in the injector prior to splitless injection is efficient but difficult to implement.
► Minimizing desorption by fast injection into cool PTV chamber is readily feasible.