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Simultaneous Determination of Trace Levels of 12 Steroid Hormones in Soil Using Modified QuEChERS Extraction Followed by Ultra Performance Liquid Chromatography–Tandem Mass Spectrometry (UPLC–MS/MS)

Ma, Shuai, Han, Ping, Li, An, Wang, Jihua, Feng, Xiaoyuan, Wang, Meng
Chromatographia 2018 v.81 no.3 pp. 435-445
androgens, chemical analysis, correlation, detection limit, edaphic factors, estrogens, liquid chromatography, progestational hormones, soil, soil sampling, steroid hormones, tandem mass spectrometry, China
Steroid hormones, mainly secreted by vertebrates, are discharged into the soil environment through surface runoff and land application of animal manure, sewage sludge, and organic fertilizers. The adequate analytical methods for steroid hormones in soil are lacking due to the requirement of rigorous sample pre-treatment. In this study, a rapid and effective modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was developed for trace simultaneous analysis of 12 steroid hormones (estrogen, androgens, and progestogens) in soil samples using ultra performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS). Samples were extracted by the mixture of acetonitrile and acetate buffer, and then cleaned with PSA/C18 absorbents. The QuEChERS method was validated by evaluating the linearity, repeatability, accuracy and precision. A suitable linear relationship was obtained in the mass concentration range of 1–100 ng g⁻¹ with high correlation coefficients (> 0.9927). The method enabled the determination of the target analytes with limits of detection between 0.0014 and 0.462 ng g⁻¹ and limits of quantification between 0.0047 and 1.54 ng g⁻¹. Soil was spiked at 5, 50 and 100 ng g⁻¹, and the recoveries ranged from 75.17 to 110.33% with relative standard deviations ≤ 9.45. The developed method was successfully applied to the analysis of soil samples collected in Beijing, and five hormones (E1, E3, αE2, And, and Tes) were detected with the concentrations ranging from 0.35 to 7.09 ng g⁻¹.