Abstract: | This work presents a new extraction material, namely, Q‐100, based on hypercrosslinked magnetic particles, which was tested in dispersive solid‐phase extraction for a group of sweeteners from environmental samples. The hypercrosslinked Q‐100 magnetic particles had the advantage of suitable pore size distribution and high surface area, and showed good retention behavior toward sweeteners. Different dispersive solid‐phase extraction parameters such as amount of magnetic particles or extraction time were optimized. Under optimum conditions, Q‐100 showed suitable apparent recovery, ranging in the case of river water sample from 21 to 88% for all the sweeteners, except for alitame (12%). The validated method based on dispersive solid‐phase extraction using Q‐100 followed by liquid chromatography with tandem mass spectrometry provided good linearity and limits of quantification between 0.01 and 0.1 μg/L. The method was applied to analyze samples from river water and effluent wastewater, and four sweeteners (acesulfame, saccharin, cyclamate, and sucralose) were found in both types of sample. |