Simultaneous determination of 15 phthalate esters in commercial beverages using dispersive liquid–liquid microextraction coupled to gas chromatography-mass spectrometry

Abstract

Phthalate esters (PAEs) are a group of endocrine disrupters that have been detected in many beverages. A simple and rapid sample pretreatment procedure based on dispersive liquid–liquid microextraction (DLLME) was performed to simultaneously extract 15 PAEs from non-alcoholic and alcoholic beverages. The extracts were analyzed using gas chromatography-mass spectrometry (GC-MS). To optimize the extraction efficiency for the 15 PAEs, various parameters, including the type and volume of extractants and dispersants, effect of salts, and extraction time were studied. Under optimum conditions, the limits of detection (LODs) and the limits of quantification (LOQs) for the 15 PAEs ranged from 0.003–0.57 ng mL⁻¹ and 0.010–1.861 ng mL⁻¹, respectively. Good linearity (0.9908 ≤ r² ≤ 0.9999) and extraction recoveries (72.6–115.5%) in the range of 0.002–0.5 μg mL⁻¹ were obtained for all selected analytes. The relative standard deviation (RSD%) for the analysis of 0.02 μg mL⁻¹ of the selected PAEs was 0.16–8.59% (n = 3). An optimized DLLME-GS-MS method was applied to detect the 15 PAEs in different beverage products, and the results demonstrated that the DLLME-GC-MS method was effective for the simultaneous analysis of 15 phthalates in beverages. The results suggest that more attention should be given to possible PAE contamination in commercial beverage products.