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采用多根整体纤维固相微萃取和液相色谱串联质谱法对水样和尿样中的全氟烷磺酸进行灵敏测定。

Sensitive determination of perfluoroalkane sulfonamides in water and urine samples by multiple monolithic fiber solid-phase microextraction and liquid chromatography tandem mass spectrometry.

机构信息

State Key Laboratory of Marine Environmental Science, Xiamen University, Xiamen 361005, China; Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystems, College of the Environment and Ecology, Xiamen University, Xiamen 361005, China.

State Key Laboratory of Marine Environmental Science, Xiamen University, Xiamen 361005, China; Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystems, College of the Environment and Ecology, Xiamen University, Xiamen 361005, China.

出版信息

Talanta. 2019 Jan 15;192:24-31. doi: 10.1016/j.talanta.2018.09.004. Epub 2018 Sep 4.

DOI:10.1016/j.talanta.2018.09.004
PMID:30348384
Abstract

To extract perfluoroalkane sulfonamides (PFASAs) in water and urine samples effectively, a new adsorbent based on poly (1H,1H,2H,2H-nonafluorohexyl acrylate/vinyboronic anhydride pyridine complex-co-ethylenedimethacrylate) monolith (FBE) was synthesized and used as the extraction phase of multiple monolithic fiber solid-phase microextraction (MMF-SPME). Because there are abundant fluorinated (F-) alkyl chains and boron atoms in the adsorbent, the FBE/MMF-SPME displays satisfactory extraction performance for PFASAs by means of fluorophilic and B-N coordination interactions. Under the most favorable conditions, the FBE/MMF-SPME was combined with HPLC-MS/MS for the sensitive monitoring of ultra-trace PFASAs in environmental water and human urine samples. The limits of detection and limits of quantification achieved for target analytes were in the range of 0.13-1.45 ng/L and 0.44-4.80 ng/L, respectively. The developed FBE/MMF-SPME-HPLC-MS/MS method was successfully applied to quantify the level of PFASAs in water and human urine samples, and ultra-trace target PFASAs were detected in the real samples. The recoveries at different fortified concentrations ranged from 80.3% to 119% with RSD in the range of 0.9-11%. Compared with reported methods, the proposed method exhibits some merits such as high sensitivity, good method precision, low consumption of sample and environmental friendliness.

摘要

为了有效地从水样和尿样中提取全氟烷磺酸 (PFASAs),合成了一种基于聚(1H,1H,2H,2H-全氟己基丙烯酸酯/乙烯基硼酸酐吡啶配合物-二乙烯基苯)整体柱的新型吸附剂,并将其用作多根整体纤维固相微萃取 (MMF-SPME) 的萃取相。由于吸附剂中含有丰富的氟化 (F-) 烷基链和硼原子,因此 FBE/MMF-SPME 通过亲氟和 B-N 配位相互作用对 PFASAs 表现出令人满意的萃取性能。在最有利的条件下,将 FBE/MMF-SPME 与 HPLC-MS/MS 结合,用于环境水样和人尿样中超痕量 PFASAs 的灵敏监测。目标分析物的检测限和定量限范围分别为 0.13-1.45ng/L 和 0.44-4.80ng/L。所开发的 FBE/MMF-SPME-HPLC-MS/MS 方法成功应用于水样和人尿样中 PFASAs 水平的定量,并在实际样品中检测到痕量目标 PFASAs。在不同加标浓度下的回收率范围为 80.3%-119%,相对标准偏差在 0.9%-11%范围内。与报道的方法相比,该方法具有灵敏度高、方法精密度好、样品和环境友好等优点。

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