An ultrahigh-performance chromatography/tandem mass spectrometry quantitative method for trace analysis of potential endocrine disrupting steroid hormones in estuarine sediments.

Rationale: Estuaries are dynamic ecosystems, providing vital habitat for unique organisms of great ecological and commercial importance. The influx of natural and synthetic steroid hormones into estuaries poses risks to these organisms and to broader ecosystem health. However, detecting these trace level pollutants in estuarine water and sediment requires improved analytical techniques.

Methods: We describe an optimized ultrahigh-performance chromatography/tandem mass spectrometry (UHPLC/MS/MS) method for simultaneous quantitation of four classes of steroid hormones (estrogens, glucocorticoids, androgens and progestins) in sediment samples collected from an Alabama estuary. Sediment samples were homogenized using Hydromatrix (HM) sorbent and extracted with methanol and water (70%, v/v). Centrifuged extracts were purified using an Agilent Bond Elut QuEChERS dispersive-SPE kit to eliminate interfering substances that could negatively influence the ionization process. Chromatographic separation was achieved on a Poroshell 120 Phenyl-Hexyl column using an Agilent 1290 Infinity II UHPLC pump. Quantitation was carried out using an Agilent triple quadrupole mass spectrometer equipped with a JetStream/ESI source in dual mode.

Results: Chromatographic separation and better peak resolution were accomplished on an Agilent Poroshell 120 Phenyl-Hexyl column using a binary gradient method with a mobile phase consisting of 1 mM ammonium fluoride in water and a mixture of methanol/acetonitrile. A dynamic multiple reaction monitoring (MRM) method was developed by optimizing various MS parameters. The method was used to analyze target steroid hormones in estuarine sediments. A total of ten steroid hormones were detected at trace amounts in estuarine sediments.

Conclusions: The optimized analytical method described here involves reasonably simple sample preparation and simultaneous trace level quantitation of four classes (estrogens, glucocorticoids, androgens and progestins) of steroid hormones in a single experimental run. Copyright © 2016 John Wiley & Sons, Ltd.