Feb 15, 2015 · The supernatant was transferred to a new HPLC vial. 100 μL of the aqueous samples were injected directly into the HPLC-MS/MS for quantification. In the HPLC-MS/MS a gradient elution consisting of methanol and Millipore water, both containing 0.2% formic acid (v/v), on a Synergi-Polar column (Phenomenex, Torrance, California, USA) was used.