The combination of two microextraction techniques (dispersive liquid-liquid microextraction [DLLME] and magnetic dispersivemicrosolid phase extraction [MDMSPE]) was developed and reported for atrazine and simazine preconcentration from wastewatersamples. The proposal methodology involved the use of magnetite supports functionalized with different alkyl or phenyl groups. Themagnetic adsorbents were synthesized by the solvothermal methodassisted by microwave, characterized, and used in the samplepreconcentration of atrazine and simazine. The method validation included parameters such as the wastewater matrix effect, repeat-ability, and recovery. The analyte separation and quantification were performed by high-performance liquid chromatography withultraviolet detection (HPLC-DAD). Parameters, such as the polarity and mass of magnetic solids and pH, were evaluated to providebetter extraction performance. The highest recoveries (> 95%) were obtained with 50 mg of the phenyl group support (CS2) at pH 5,using 5 mL of the sample and carbon tetrachloride and methanol, as extraction and dispersive solvents, respectively. The lowest limitsof detection (LOD) achieved were 13.16 and 13.86 ng L−1, and the limits of quantification (LOQ) were 43.89 and 46.19 ng L−1forsimazine and atrazine, respectively, with repeatability (expressed as %RSD) below 5% in all cases. The developed method is simple,easy, and low cost for the analysis of two herbicides potentially dangerous for environmental and human health.
