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In this research paper, we report a method able to detect perfluorinated compound at pg·L−1 levels in superficial and underground water samples. An online solid phase extraction HPLC-MS/MS method was developed for the analysis of 12 perfluoroalkyl acids (PFASs). The method is based on injection of 5000 µL of water sample in SPE online WAX column followed by chromatography separation and mass spectrometry determination. SPE online elution was performed by water + 0.05% NH4OH and methanol + 0.05% NH4OH, while separation of target compounds was achieved within 10 min by Gemini chromatographic column operating from 1 to 12 pH range and using a mixture of water-methanol + 0.05% NH4OH. Sub ng·L−1 method detection limits (from 0.2 to 5 ng·L−1), linearity (from 0.2 to 250 ng·L−1), accuracy (from 80 to 120%), and precision (RSD less than 15% at LOQs levels) were achieved. The method is capable of measuring PFAS at trace levels, but above all it can reach the limit of 200 pg·L−1 required by European regulation for PFOS determination in surface and underground waters. The method was validated for quantitative analysis of PFASs in real water samples.

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