A method for the trace analysis of polar micropollutants (MPs) by direct injection of surface water and groundwater was validated with ultrahigh-performance liquid chromatography using a core-shell biphenyl stationary phase coupled to time-of-flight high-resolution mass spectrometry. The validation was successfully conducted with 33 polar MPs representative for several classes of emerging contaminants. Identification and quantification were achieved by semi-automated processing of full-scan and data-independent acquisition MS/MS spectra. In most cases good linearity (R² ≥ 0.99), recovery (75% to 125%) and intra-day (RSD < 20%) and inter-day precision (RSD < 10%) values were observed. Detection limits of 9 to 83 ng/L and 9 to 93 ng/L could be achieved in riverbank filtrate and surface water, respectively. A solid-phase extraction was additionally validated to screen samples from full-scale reverse osmosis drinking water treatment at sub-ng/L levels and overall satisfactory analytical performance parameters were observed for RBF and reverse osmosis permeate. Applicability of the direct injection method is shown for surface water and riverbank filtrate samples from an actual drinking water source. Several targets linkable to incomplete removal in wastewater treatment and farming activities were detected and quantified in concentrations between 28 ng/L for saccharine in riverbank filtrate and up to 1 μg/L for acesulfame in surface water. The solid phase extraction method applied to samples from full-scale reverse osmosis drinking water treatment plant led to quantification of 8 targets between 6 and 57 ng/L in the feed water, whereas only diglyme was detected and quantified in reverse osmosis permeate. Our study shows that combining the chromatographic resolution of biphenyl stationary phase with the performance of time-of-flight high-resolution tandem mass spectrometry resulted in a fast, accurate and robust method to monitor polar MPs in source waters by direct injection with high efficiency.

通过使用核壳联苯固定相与飞行时间高分辨率质谱联用的超高效液相色谱法，验证了通过直接注入地表水和地下水来痕量分析极性微污染物（MPs）的方法。验证是由33位极性MP代表的几类新兴污染物进行的。鉴定和定量通过全扫描和数据独立的采集MS / MS光谱的半自动化处理来实现。在大多数情况下，良好的线性度（R ²≥0.99），回收率（75％至125％）和日内（RSD <20％）和日间精度（RSD <10％）值均被观察到。在河岸滤液和地表水中，检出限分别为9到83 ng / L和9到93 ng / L。此外，还对固相萃取进行了验证，以从亚ng / L浓度的全规模反渗透饮用水处理中筛选样品，并且观察到了令人满意的RBF和反渗透透过物总体分析性能参数。显示了直接进样方法对来自实际饮用水源的地表水和河岸滤液样品的适用性。检测并确定了与废水处理和农业活动中的不完全清除有关的几个目标，并确定了其浓度，其中河岸滤液中的糖精浓度为28 ng / L，地表水中的乙酰磺胺酸浓度最高为1μg/ L。固相萃取法应用于全尺寸反渗透饮用水处理厂的样品，导致进水中8个目标样品的定量在6到57 ng / L之间，而在反渗透渗透物中仅检测到了二甘醇二甲醚并对其进行了定量。我们的研究表明，联苯固定相的色谱分离度与飞行时间高分辨率串联质谱的性能相结合，导致了一种快速，准确和鲁棒的方法，可以通过直接注入高效地监测水源中的极性MP。固相萃取法应用于全尺寸反渗透饮用水处理厂的样品，导致进水中8个目标样品的定量在6到57 ng / L之间，而在反渗透渗透物中仅检测到了二甘醇二甲醚并对其进行了定量。我们的研究表明，联苯固定相的色谱分离度与飞行时间高分辨率串联质谱的性能相结合，导致了一种快速，准确和鲁棒的方法，可以通过直接注入高效地监测水源中的极性MP。固相萃取法应用于全尺寸反渗透饮用水处理厂的样品，导致进水中8个目标样品的定量在6到57 ng / L之间，而在反渗透渗透物中仅检测到了二甘醇二甲醚并对其进行了定量。我们的研究表明，联苯固定相的色谱分离度与飞行时间高分辨率串联质谱的性能相结合，导致了一种快速，准确和鲁棒的方法，可以通过直接注入高效地监测水源中的极性MP。