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This service provides a sensitive and rapid method for the simultaneous analysis of artificial sweeteners, aspartame, acesulfame, cyclamate, saccharine, and phenylalanine in water samples using solid-phase and large-volume sample stacking-capillary electrophoresis (SPE-LVSS-CE). Under optimal conditions, the method had a linear range of 0.08 to 2.0 mg L−1, with limits of detection ranging from 0.03 to 0.18 mg L−1 with inter- and intraday repeatabilities < 10% (as a relative standard deviation) in all cases. The SPE-LVSS-CE is a robust, easy, fast, and efficient strategy for online preconcentration of artificial sweeteners in complex matrices.