Guedes-Alonso Rayco, Santana-Viera Sergio, Montesdeoca-Esponda Sarah, Afonso-Olivares Cristina, Sosa-Ferrera Zoraida, Santana-Rodríguez José Juan
Instituto Universitario de Estudios Ambientales y Recursos Naturales (i-UNAT), Universidad de Las Palmas de Gran Canaria, Campus Universitario de Tafira, 35017, Las Palmas de Gran Canaria, Spain.
Anal Bioanal Chem. 2016 Sep;408(24):6833-44. doi: 10.1007/s00216-016-9810-7. Epub 2016 Aug 8.
Hormonal compounds are a concern to the international community because they can affect the aquatic biota and are therefore considered to be endocrine-disrupting compounds. These compounds have lipophilic properties, so they tend to accumulate in solid matrices, such as sewage sludge. This work presents the optimization of a microwave-assisted extraction process combined with ultra-high performance liquid chromatography-tandem mass spectrometry for the determination of 15 hormonal compounds in sludge samples. The proposed method has relative standard deviations below 23 %, good recoveries (over 71 %) for all compounds, detection limits that ranged from 1.1 to 7.9 ng g(-1) and quantification limits which ranged from 3.7 to 26.3 ng g(-1). The method was used to analyse sludge samples from four different wastewater treatment plants of Gran Canaria (Spain) with different wastewater treatments. 17β-estradiol, 17α-ethynylestradiol, norgestrel and cortisone were detected in sludge samples at concentrations that ranged from 17.3 to 1.44 × 10(3) ng g(-1). The developed method permits the use of small quantities of sample and organic solvents, presents short extractions times and is the first one based on microwave-assisted extraction for the analysis of both sex hormones and corticosteroids.
激素化合物受到国际社会的关注,因为它们会影响水生生物群,因此被视为内分泌干扰化合物。这些化合物具有亲脂性,所以它们倾向于在固体基质(如污水污泥)中积累。这项工作展示了一种微波辅助萃取过程与超高效液相色谱 - 串联质谱联用的方法优化,用于测定污泥样品中的15种激素化合物。所提出的方法相对标准偏差低于23%,所有化合物的回收率良好(超过71%),检测限在1.1至7.9 ng g⁻¹之间,定量限在3.7至26.3 ng g⁻¹之间。该方法用于分析来自西班牙大加那利岛四个不同污水处理厂且采用不同废水处理方式的污泥样品。在污泥样品中检测到17β - 雌二醇、17α - 乙炔雌二醇、炔诺孕酮和可的松,浓度范围为17.3至1.44×10³ ng g⁻¹。所开发的方法允许使用少量样品和有机溶剂,萃取时间短,并且是首个基于微波辅助萃取用于分析性激素和皮质类固醇的方法。