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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)

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Abstract

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.

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Acknowledgements

The present work was funded by the Open Project of the Risk Assessment Lab for Agro-products (Beijing) Ministry of Agriculture (ZBZXKFKT201503), Open Project of the Risk Assessment Lab for Agro-products (Beijing) Ministry of Agriculture (ZBZXKFKT201701) and Special projects of construction of science and technology innovation ability of Beijing academy of agriculture and forestry sciences (KJCX20150408).

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Authors and Affiliations

  1. Beijing Research Center for Agricultural Standards and Testing, No. 9 Middle Road of Shu Guang Hua Yuan, Haidian Dist., Beijing, 100097, China

    Shuai Ma, Ping Han, An Li, Jihua Wang, Xiaoyuan Feng & Meng Wang

  2. Risk Assessment Laboratory for Agro-Products (Beijing), Ministry of Agriculture, No. 9 Middle Road of Shu Guang Hua Yuan, Haidian Dist., Beijing, 100097, China

    Shuai Ma, Ping Han, An Li, Jihua Wang, Xiaoyuan Feng & Meng Wang

  3. Beijing Municipal Key Laboratory of Agriculture Environment Monitoring, No. 9 Middle Road of Shu Guang Hua Yuan, Haidian Dist., Beijing, 100097, China

    Shuai Ma, Ping Han, An Li, Jihua Wang, Xiaoyuan Feng & Meng Wang

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  1. Shuai Ma
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Ma, S., Han, P., Li, A. et al. 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). Chromatographia 81, 435–445 (2018). https://doi.org/10.1007/s10337-017-3464-2

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