Santos Lúcia H M L M, Ramalhosa Maria João, Ferreira Marta, Delerue-Matos Cristina
REQUIMTE/LAQV/Instituto Superior de Engenharia do Instituto Politécnico do Porto, Rua Dr. António Bernardino de Almeida, 431, 4200-072 Porto, Portugal; CIIMAR/CIMAR-Interdisciplinary Centre of Marine and Environmental Research, Coastal and Marine Environmental Toxicology Group, University of Porto, Rua dos Bragas, 289, 4050-123, Portugal.
REQUIMTE/LAQV/Instituto Superior de Engenharia do Instituto Politécnico do Porto, Rua Dr. António Bernardino de Almeida, 431, 4200-072 Porto, Portugal.
J Chromatogr A. 2016 Mar 11;1437:37-48. doi: 10.1016/j.chroma.2016.01.079. Epub 2016 Feb 4.
An analytical method based on a modified Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) extraction procedure followed by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed for the analysis of psychiatric drugs in sediments. An optimized approach was applied in sample preparation by using basic acetonitrile as extraction solvent. Extraction was followed by a clean-up using dispersive solid phase extraction (dSPE) to remove matrix interfering compounds. The analytical method was validated in terms of sensitivity, linearity, recovery, intra- and inter-day precisions and method detection and quantification limits. Under optimized conditions, limits of detection ranged from 0.01ngg(-1) to 2.08ngg(-1); and recoveries between 47 and 110% with relative standard deviation (RSD) below 5%. The developed methodology was applied to sediments of two Portuguese rivers (Douro and Lima rivers) and nine out of eleven psychiatric drugs were detected in sediments at concentrations up to 26.4ngg(-1) (dry weight). To the best of our knowledge, it was the first time that the human metabolites norfluoxetine and norsertraline were detected in river sediments at levels of few nanograms per gram.
建立了一种基于改进的快速、简便、廉价、高效、耐用和安全（QuEChERS）萃取方法，随后采用超高效液相色谱-串联质谱（UHPLC-MS/MS）的分析方法，用于分析沉积物中的精神类药物。通过使用碱性乙腈作为萃取溶剂，在样品制备中应用了优化方法。萃取后采用分散固相萃取（dSPE）进行净化，以去除基质干扰化合物。该分析方法在灵敏度、线性、回收率、日内和日间精密度以及方法检测限和定量限方面进行了验证。在优化条件下，检测限范围为0.01ng g(-1)至2.08ng g(-1)；回收率在47%至110%之间，相对标准偏差（RSD）低于5%。所开发的方法应用于葡萄牙两条河流（杜罗河和利马河）的沉积物，在沉积物中检测到11种精神类药物中的9种，浓度高达26.4ng g(-1)（干重）。据我们所知，这是首次在河流沉积物中检测到纳克每克水平的人体代谢物去甲氟西汀和去甲舍曲林。
