A rapid and reliable method enabling high-throughput sample analysis for quicker data generation, detection, and monitoring of eight selected steroid hormones in water matrixes was developed and validated. Our approach is based on a novel sample introduction method, the laser diode thermal desorption/atmospheric pressure chemical ionization (LDTD/APCI) coupled to tandem mass spectrometry (MS/MS). The optimization of instrumental parameters and a method application are presented. Our method was successfully applied to spiked effluent wastewater in the low-nanogram per liter concentrations with total analysis time reduced to seconds (15 s) using LDTD/APCI-MS/MS compared to minutes with traditional liquid-chromatography coupled to tandem mass spectrometry (LC-MS/MS) following solid-phase extraction (SPE). The instrumental detection limits for LDTD/APCI-MS/MS ranged from 5 to 24 microg L(-1) and from 13 to 43 ng L(-1) for the method detection limits. Calibration curves in wastewater matrix showed good linearity (R(2) > 0.99), and precision (intraday and interday) was below 20%. This work demonstrates that LDTD/APCI-MS/MS could be used for fast and effective quantitative analysis of emerging contaminants in different water matrixes with reduced cost by eliminating the chromatography step used in traditional LC-MS/MS.

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BackgroundIn recent years, endocrine disrupting compounds (EDCs) have been found in rivers that receive significant inputs of wastewater. Among EDCs, natural and synthetic steroid hormones are recognized for their potential to mimic or interfere with normal hormonal functions (development, growth and reproduction), even at ultratrace levels (ng L−1). Although conjugated hormones are less active than free hormones, they can be cleaved and release the unconjugated estrogens through microbial processes before or during the treatment of wastewater. Due to the need to identify and quantify these compounds, a new fully automated method was developed for the simultaneous determination of the two forms of several steroid hormones (free and conjugated) in different water matrixes and in urine.ResultsThe method is based on online solid phase extraction coupled with liquid chromatography and tandem mass spectrometry (SPE–LC–MS/MS). Several parameters were assessed in order to optimize the efficiency of the method, such as the type and flow rate of the mobile phase, the various SPE columns, chromatography as well as different sources and ionization modes for MS. The method demonstrated good linearity (R2 > 0.993) and precision with a coefficient of variance of less than 10 %. The quantification limits vary from a minimum of 3–15 ng L−1 for an injection volume of 1 and 5 mL, respectively, with the recovery values of the compounds varying from 72 to 117 %.ConclusionThe suggested method has been validated and successfully applied for the simultaneous analysis of several steroid hormones in different water matrixes and in urine.Electronic supplementary materialThe online version of this article (doi:10.1186/s13065-016-0174-z) contains supplementary material, which is available to authorized users.

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