A new analytical method was developed to extract and determine 25 perfluorinated and polyfluorinated alkyl substances from aqueous samples using an automated solid phase extraction system and liquid chromatography–tandem mass spectrometry. Full method validation including assessment of background signal, lowest concentration minimum reporting level, calibration, limit of quantitation, precision, and accuracy was performed. The analysis of drinking water samples was performed for all target analytes. This method also incorporates the use of isotope dilution in which isotopically labeled analogs of the target analytes are added to the sample prior to extraction in a known amount to correct for sample matrix interference and improve data quality. We demonstrated that the automated solid‐phase extraction system provided reliable extraction of the target perfluorinated and polyfluorinated alkyl substances analytes from large‐ of use, reduced human errors, avoidance of massive lab contaminations and saving up to 50% operational time to manual operation while ensuring high reproducibility and productivity for analytical testing laboratories.
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