A new, simple, fast and high sensitive analytical method based on dispersive liquid-liquid microextraction (DLLME) followed by gas chromatography-mass spectrometry (GC-MS) for the simultaneous determination of nitro musks in surface water and wastewater samples is presented. Different parameters, such as the nature and volume of both the extraction and disperser solvents and the ionic strength and pH of the aqueous donor phase, were optimized. Under the selected conditions (injection of a mixture of 1 mL of acetone as disperser solvent and 50 μL of chloroform as extraction solvent, no salt addition and no pH adjustment) the figures of merit of the proposed DLLME-GC-MS method were evaluated. High enrichment factors, ranging between 230 and 314 depending on the target analyte, were achieved, which redound to limits of detection in the ng L(-1) range (i.e., 4-33 ng L(-1)). The relative standard deviation (RSD) was below 5% for all the target analytes. Finally, the recoveries obtained for different water samples of diverse origin (sea, river, irrigation channel and water treatment plant) ranged between 87 and 116%, thus showing no matrix effects.
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