Pristine humic acids (HAs) were thermally condensed onto silica microparticles by a one-pot, inexpensive and green preparation route obtaining a mixed-mode sorbent ([email protected]) with good sorption affinity for glucocorticoids (GCs). The carbon-based material, characterized by various techniques, was indeed applied as the sorbent for fixed-bed solid-phase extraction of eight GCs from river water and wastewater treatment plant effluent, spiked at different concentration levels in the range 1–400 ng L⁻¹. After sample extraction, the target analytes were simultaneously and quantitatively eluted in a single fraction of methanol, achieving enrichment factor 4000 and 1000 in river water and wastewater effluent, respectively. Full recovery for all compounds, was gained in the real matrices studied (80–125% in river water, 79–126% in wastewater effluent), with inter-day precision showing relative standard deviations (RSD) below 15% and 18% (n = 3), for river and wastewater effluent, correspondingly. The high enrichment factors coupled with high-performance liquid chromatography tandem mass spectrometry quantification (MRM mode) provided method quantification limits of 0.009–0.48 ng L⁻¹ in river water and 0.06–3 ng L⁻¹ in wastewater effluent and, at the same time, secure identification of the selected drugs. As also evidenced by comparison with literature, [email protected] proved to be a valid alternative to the current commercial sorbents, in terms of extraction capability, enrichment factor, ease of preparation and cost. The batch-to-batch reproducibility was assessed by recovery tests on three independently prepared [email protected] powders (RSD lower than 7%).

通过一锅，廉价和绿色的制备路线，将原始的腐殖酸（HAs）热缩到二氧化硅微粒上，从而获得对糖皮质激素（GCs）具有良好吸附亲和力的混合模式吸附剂（[电子邮件保护]）。实际上，以各种技术为特征的碳基材料已被用作吸附剂，用于固定床固相萃取从河水和废水处理厂废水中提取的八种气相色谱仪，其浓度范围为1–400 ngL。^-1。样品提取后，将目标分析物同时并定量地洗脱在甲醇的单个馏分中，分别在河水和废水中获得富集系数4000和1000。在所研究的实际基质中，所有化合物均得到了完全回收（在河水中为80–125％，在废水中为79–126％），日间精度显示相对标准偏差（RSD）分别低于15％和18％（n  = 3），分别对应于河流和废水排放。加上纳克升0.009-0.48高效液相色谱-串联质谱定量（MRM模式）提供的方法定量限高富集因子^-1在河水和0.06-3纳克大号^-1废水，并同时确保所选药物的安全鉴定。从与文献的比较中也可以看出，就提取能力，富集系数，制备简便性和成本而言，[电子邮件保护]已被证明是当前商业吸附剂的有效替代品。通过对三种独立制备的[受电子邮件保护的]粉末（RSD低于7％）进行回收率测试，评估了批次间的可重复性。