Development of a multi-hormone analysis method by LC-MS/MS for environmental water application using diffusive gradient in thin films
2022
Martins de Barros, Rachel | Lissalde, Sophie | Guibal, Robin | Guibaud, Gilles
An analysis method for four families of hormones (estrogens, progestins, androgens and prostaglandins), dedicated to an efficient water monitoring with passive sampling, was developed using a liquid chromatography tandem mass spectrometry with triple quadrupole coupling and universal electrospray ionisation. Thirteen natural and synthetic hormones in ultra-pure water could be analysed in a single run according to the French Standard NF T90-210: calibration range of 0.1 (except for 17β-Estradiol, Estriol, Estrone and Diethylstilbestrol, from 0.5 μg/L; and Ethinylestradiol, from 1 μg/L) to 20 μg/L with linear regressions (R² ≥ 0.96), maximum accuracy deviations of 30% at intermediate fidelity for three concentration references (1, 10 and 20 μg/L) and instrumental LOQs from 0.05 to 1 μg/L. The stability of 11 hormones (10 μg/L) was studied under several storage conditions and sample evaporation. All selected hormones were stable for 60 days at −18 °C, 7 days at 4 °C and 7 days at 20 °C but continued drying flow after evaporation should be avoided, especially for 17α-Estradiol, Estrone and Diethylstilbestrol. Observed matrix effects using o-DGT extracts (diffusive gradient in thin-film sampler for polar organics) containing an environmental matrix varied from 24 to 92% but all matrix effects were corrected with IS use. Therefore, the developed method, coupled with o-DGT, was tested with the o-DGT deployment in rivers. Using diffusion coefficients from the literature or lab determined, the concentrations in the rivers varied for Estrone from 1.8 ng/L to 2.5 ng/L, and for Androstenedione from 0.4 to 1.1 ng/L.
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