水体中17种持久性和可迁移有机污染物的检测

持久性和移动性有机污染物 (persistent and mobile organic contaminants, PMOCs) 在环境中降解缓慢，并且可以通过水体循环进行迁移。由于缺乏水体中PMOCs的高效富集和准确测定方法，导致关于PMOCs在水体中存在水平的可靠监测数据较少。通过优化固相萃取条件和高效液相色谱-串联质谱参数，建立了同时检测水中17种PMOCs的分析方法。采用HLB固相萃取柱对水样中的PMOCs进行富集，乙腈和含10 mmol·L⁻¹乙酸铵的水溶液作为流动相进行梯度洗脱，PMOCs检出限为0.04~0.35 ng·L⁻¹，定量限为0.13~1.16 ng·L⁻¹，回收率为65.01%~98.65%。在北京潮白河、广东北江和河北滹沱河进行布点采样，并测定其PMOCs的质量浓度。实验结果表明：17种PMOCs在潮白河、北江和滹沱河中均有检出，其ƩPMOCs平均质量浓度分别为604.69、740.45和505.11 ng·L⁻¹。潮白河地表水中安赛蜜、金刚烷胺和己内酰胺的质量浓度相对较高，分别高达261.75、143.84和153.71 ng·L⁻¹。北江中安赛蜜、磷酸三 (2-氯丙基) 酯和己内酰胺的质量浓度相对较高，分别高达433.14、444.46和108.76 ng·L⁻¹。滹沱河中金刚烷胺、己内酰胺和磷酸三 (2-氯丙基) 酯的质量浓度较高，分别高达218.10、101.14和222.60 ng·L⁻¹。本研究结果可为地表水和地下水水体中PMOCs的检测评价提供参考。

Determination of 17 persistent and mobile organic contaminants (PMOCs) in water

The persistent and mobile organic contaminants (PMOCs) in aquatic environments degrade very slowly and present a great ability to spread through the water cycle. Due to the lack of both enrichment and determination methods for PMOCs analysis in water samples, only a few reliable monitoring data as regards the real levels of these compounds. The analytical methods were developed to determine 17 PMOCs in the surface and ground water with solid-phase extraction (SPE) pretreatment and liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Water samples were concentrated by SPE with the HLB cartridge, and gradient elution was performed using methanol and 10 mmol·L−1 ammonium acetate as the mobile phases. The limits of detection (LODs) and quantitation (LOQs) for the 17 PMOCs ranged from 0.04~0.35 ng·L−1 and 0.13~1.16 ng·L−1, respectively. The average recoveries of the 17 PMOCs ranged from 65.01%~98.65%. Water samples were collected and detected from Chaobai River (Beijing), Beijiang River (Guangdong) and Hutuo River (Hebei). The average concentrations of ƩPMOCs were respectively 604.69, 740.45 and 505.11 ng·L−1. The concentrations of acesulfame, amantadine and caprolactam in the Chaobai River were relatively high, as high as 261.75, 143.84 and 153.71 ng·L−1. The concentrations of acesulfame, tris(1-chloro-2-propyl) phosphate and caprolactam in the Chaobai River were relatively high, as high as 433.14, 444.46, 108.76 ng·L−1. The concentrations of amantadine, caprolactam and tris(1-chloro-2-propyl) phosphate in the Hutuo River were relatively high, as high as 218.10, 101.14 and 222.60 ng·L−1. This study can provide a reference for the detection assessment of PMOCs in surface water and groundwater.