Department of Chemistry, Sapienza University, P.le Aldo Moro 5, Rome 00185, Italy.
Department of Chemistry, Sapienza University, P.le Aldo Moro 5, Rome 00185, Italy.
J Chromatogr A. 2020 Jun 21;1621:461080. doi: 10.1016/j.chroma.2020.461080. Epub 2020 Apr 11.
This paper describes a procedure for the isolation of 20 organic micro-pollutants among pesticides, drugs, recreational drugs, flame retardants from river sediments. After a solid-liquid extraction with a methanol:water (50:50, v/v) solution, the supernatant was diluted with water and cleaned up by stir-disc solid-phase extraction (SPE). The disc was made of buckypaper, a self-supporting entangled assembly of carbon nanotubes, which was used as a highly porous, two-sided, sorbent membrane. In the preliminary activation step, the membrane was oxidised for 2-hours with nitric acid to extend its extraction capability also to more polar compounds. All extracts were analysed by ultra-high-performance liquid chromatography-tandem mass spectrometry. A comparative investigation with commercial Strata-X Polymeric Reversed Phase SPE cartridges proved the effectiveness of the lab-made device. On the average, the analytes were recovered with yields around 69% (low spike level) and 80% (medium and high spike level), while only a couple of analytes exhibited values less than 50%. The relative standard deviation was always less than 20%. Limits of detections were in the range 0.02-9.9 ng g. The validated method was then applied for the analysis of sediment samples from different sites of the River Turia basin in the area of Valencia (Spain), finding tris(2-chloroisopropyl)-phosphate in all sediments at a level ranging from 6.9 to 387.9 ng g. Other compounds, such as pesticides and pharmaceuticals were more sporadically in these samples.
本文描述了一种从河底沉积物中分离 20 种有机微量污染物（包括农药、药物、娱乐性毒品和阻燃剂）的方法。采用甲醇：水（50:50，v/v）溶液进行固液萃取后，将上清液用稀释水稀释，并用搅拌盘固相萃取（SPE）进行净化。该圆盘由 buckypaper 制成，buckypaper 是一种由碳纳米管自支撑缠结组装而成的高度多孔、双面吸附剂膜。在初步的活化步骤中，将膜用硝酸氧化 2 小时，以扩展其对更极性化合物的提取能力。所有提取物均采用超高效液相色谱-串联质谱法进行分析。与商业 Strata-X 聚合型反相 SPE 小柱的对比研究证明了实验室自制设备的有效性。平均而言，分析物的回收率在低加标水平下约为 69%，在中高加标水平下约为 80%，而只有少数几种分析物的回收率低于 50%。相对标准偏差始终小于 20%。检测限范围为 0.02-9.9ng g。验证后的方法随后应用于分析瓦伦西亚（西班牙）图里亚河流域不同地点的沉积物样品，在所有沉积物中均发现三（2-氯异丙基）磷酸酯的含量在 6.9 至 387.9ng g 之间。其他化合物，如农药和药物，在这些样品中更为零星。
