Department of Environmental Chemistry, IDAEA-CSIC, C/Jordi Girona 18-26, 08034 Barcelona, Spain.
Chemosphere. 2011 Nov;85(8):1390-9. doi: 10.1016/j.chemosphere.2011.07.071. Epub 2011 Oct 6.
This work describes the development, optimization and validation of an analytical method for the simultaneous detection and identification of 74 pharmaceutically active compounds (PhACs), from various therapeutic groups, in both environmental (ground and surface water) and wastewaters (WW). The method is based on the simultaneous extraction of all target compounds by solid phase extraction (SPE), using a hydrophilic-lipophilic balanced polymer followed by ultra high performance liquid chromatography (UHPLC) tandem mass spectrometry (MS/MS). Two selected reaction monitoring (SRM) transitions have been monitored per compound in order to fulfil the EC guidelines, as well as to ensure an accurate identification of target compounds in the samples. Quantification is performed by internal standard approach, applying 24 specific isotopically labeled compounds. The main advantages of the developed method, besides the selectivity and reliability of the results, is its high throughput. All compounds are extracted in a single step and the instrumental analysis lasts 5 min (NI mode)+8 min (PI mode), allowing fast throughput of samples. The limits of detection range from 0.01 to 50 ng L(-1), depending on the matrix, for most of the compounds. Finally, the method developed has been applied to the analysis of pharmaceuticals in the Ebro river basin (NE Spain).
本工作描述了一种分析方法的开发、优化和验证，该方法可用于同时检测和鉴定来自不同治疗组的 74 种药物（PhACs），包括环境（地下水和地表水）和废水中的药物（WW）。该方法基于固相萃取（SPE）对所有目标化合物进行同时提取，使用亲水-亲脂平衡聚合物，然后进行超高效液相色谱（UHPLC）串联质谱（MS/MS）分析。为了满足欧盟委员会的指导方针，并确保对样品中目标化合物进行准确鉴定，每个化合物监测两个选择反应监测（SRM）转换。通过内标法进行定量分析，应用 24 种特定的同位素标记化合物。除了结果的选择性和可靠性外，该方法的主要优点是其高通量。所有化合物都可以在单个步骤中提取，仪器分析耗时 5 分钟（NI 模式）+8 分钟（PI 模式），允许快速处理样品。大多数化合物的检测限范围为 0.01 至 50ng/L，具体取决于基质。最后，该方法已应用于西班牙东北部埃布罗河流域的药物分析。
