Trace determination of prohibited acrylamide in cosmetic products by vortex-assisted reversed-phase dispersive liquid-liquid microextraction and liquid chromatography-tandem mass spectrometry

Abstract

An analytical method for the determination of residual acrylamide in cosmetic products containing potential acrylamide-releasing ingredients is presented. The method is based on vortex-assisted reversed-phase dispersive liquid-liquid microextraction (VA-RP-DLLME) to extract and preconcentrate acrylamide by using water as extraction solvent taking advantage the highly polar behavior of this analyte, followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) for its determination. Under optimized conditions (5 mL toluene as supporting solvent, 50 µL of water as extraction solvent, 1 min for vortex extraction time) the method was properly validated obtaining good analytical features (linearity up to 20 ng mL−1, method limits of detection and quantification of 0.51 and 1.69 ng g−1, respectively, enrichment factor of 52, and good repeatability (RSD < 4.1%)). The proposed analytical method was applied to the determination of acrylamide in commercial samples that were weighed and dispersed in the minimum quantity of methanol (50 µL) by vortex stirring before applying the VA-RP-DLLME procedure. Through the pretreatment of the sample and the use of acrylamide-d3 as surrogate, the matrix effect was overcome, obtaining good relative recovery values (88–108%). The proposed method has shown efficacy, simplicity, and speed, and it allows the determination of acrylamide at trace levels easily, which could make it very useful for companies in the quality control of cosmetic products containing potential acrylamide-releasing ingredients to fulfill the safety limits imposed by European Regulation.