ASE-UHPLC-MS/MS Determination of 8 Environmental Endocrine Disrupters in Sediments

The pretreated sediment sample (5.000 g) was mixed thoroughly with neutral Al₂O₃ (25 g), and 8 endocrine disrupters in the sample were separated by ASE as described with a mixture of acetone and methanol (1+1). The extract was concentrated to 2 mL by N₂-blowing, 400 mL of water were added and acidity of the solution was adjusted to pH 3. The solution was then purified by passing through HLB-SPE column. After drying the column by N₂-blowing, it was eluted with 8 mL of acetone. The treated eluate was separated by UHPLC using BEH C₁₈ column as the stationary phase, and mixtures of methanol and 0.1% (φ) ammonia solution, mixed in various volumic ratios, as mobile phase in gradient elution. ESI^- and MRM were adopted in MS. Linear relationships between values of peak area and mass concentration of 8 compounds were found in the range of 2.0-100.0 μg·L^-1, with detection limits (3s) in the range of 0.03-0.05 μg·kg^-1. Test for recovery was made by standard addition method at 3 concentration levels, giving results in the range of 62.8%-104%, with RSDs (n=6) ranged from 2.8% to 15%.