Previous studies on organic sediment contaminants focused mainly on a limited number of highly hydrophobic micropollutants accessible to gas chromatography using nonpolar, aprotic extraction solvents. The development of liquid chromatography–high-resolution mass spectrometry (LC–HRMS) permits the spectrum of analysis to be expanded to a wider range of more polar and ionic compounds present in sediments and allows target, suspect, and nontarget screening to be conducted with high sensitivity and selectivity. In this study, we propose a comprehensive multitarget extraction and sample preparation method for characterization of sediment pollution covering a broad range of physicochemical properties that is suitable for LC–HRMS screening analysis. We optimized pressurized liquid extraction, cleanup, and sample dilution for a target list of 310 compounds. Finally, the method was tested on sediment samples from a small river and its tributaries. The results show that the combination of 100 °C for ethyl acetate–acetone (50:50, neutral extract) followed by 80 °C for acetone–formic acid (100:1, acidic extract) and methanol–10 mM sodium tetraborate in water (90:10, basic extract) offered the best extraction recoveries for 287 of 310 compounds. At a spiking level of 1 μg mL^-1, we obtained satisfactory cleanup recoveries for the neutral extract—(93 ± 23)%—and for the combined acidic/basic extracts—(42 ± 16)%—after solvent exchange. Among the 69 compounds detected in environmental samples, we successfully quantified several pharmaceuticals and polar pesticides.

先前对有机沉积物污染物的研究主要集中在有限数量的高度疏水性微污染物上，这些污染物可通过使用非极性，非质子萃取溶剂的气相色谱法获得。液相色谱-高分辨率质谱（LC-HRMS）的发展使分析范围扩大到沉积物中存在的更多极性和离子性化合物，并可以使用高灵敏度和选择性。在这项研究中，我们提出了一种用于表征沉积物污染的全面的多目标提取和样品制备方法，该方法涵盖了广泛的理化性质，适用于LC–HRMS筛选分析。我们优化了加压液体的提取，净化，和样品稀释以得到310种化合物的目标清单。最后，该方法在一条小河及其支流的沉积物样品上进行了测试。结果表明，乙酸乙酯-丙酮（50:50，中性提取物）在100°C的条件下，丙酮-甲酸（100：1，酸性提取物）和甲醇–10 mM四硼酸钠的水溶液在80°C的组合（90:10，基本提取物）为310种化合物中的287种提供了最佳的提取回收率。加标浓度为1μgmL 碱性提取物）为310种化合物中的287种提供了最佳的提取回收率。加标浓度为1μgmL 碱性提取物）为310种化合物中的287种提供了最佳的提取回收率。加标浓度为1μgmL^-1，我们在溶剂交换后获得了中性提取物（（93±23）％）和组合的酸性/碱性提取物（（42±16）％）的令人满意的净化回收率。在环境样品中检测到的69种化合物中，我们成功地定量了几种药物和极性农药。