A multiresidue method for the simultaneous quantification of 72 micropollutants in aqueous samples by ultra high performance liquid chromatography–high resolution mass spectrometry (UHPLC–HRMS) is described. A variety of substance classes like industrial chemicals, analgesics, anticonvulsants, antihypertensives, psychoactive substances, flame retardants, neutral and acidic pesticides are comprised. A sample volume of 1 mL was enriched by online solid phase extraction (SPE), separated on a 2.6 μm core–shell column and detected with an Exactive™ high resolution mass spectrometer. Simultaneous determination of compounds with different ionization behavior was achieved by polarity switching. One complete run lasted 15 min. The method was validated in the matrices drinking water (DW), diluted surface water (dSW) and diluted waste water treatment plant effluent (dWW) by analyzing 10 replicates spiked at two concentration levels. Limits of quantification (LOQs) ranged between 0.01 and 0.06 μg/L in DW, 0.03 and 0.38 μg/L in dSW, 0.06 and 0.38 μg/L in dWW. The accuracies were between 77 and 117% in DW, 70 and 121% in dSW, 71 and 121% in dWW for both spike levels, respectively. Five compounds in dSW and one compound in dWW were affected by matrix effects, leading to accuracies outside the ranges stated above. The precision for level 2 was excellent with relative standard deviations (RSDs) between 2.2 and 6.5% in DW, 0.5 and 4.9% in dSW and between 1.2 and 6.6% in dWW.

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