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


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. Electronic address: [Email]


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.


Boronate affinity,Fluorophilicity,Perfluoroalkane sulfonamides,Solid-phase microextraction,Urine,Water,