Preparation of superhydrophobic magnetic Fe₃O₄@C16&TMS nanomaterials and their application to the determination of eight volatile methylsiloxanes in water

A superhydrophobic magnetic nanomaterial, Fe 3 O 4 @C16&TMS, was synthesized by hexadecylating the surface of the Fe₃O₄ nanoparticles and sealing the residual hydroxyl groups. The nanomaterial exhibits a high specific surface area of 45.3 m²/g, and superhydrophobicity with a water contact angle of 158.11°. The high specific surface area offers numerous adsorption sites, and the superhydrophobic characteristics of the synthesized nanomaterial can selectively enrich non-polar volatile methylsiloxanes (VMSs) through hydrophobic interactions, thereby significantly enhancing extraction efficiency and reducing matrix interference. Notably, no significant decline in performance was observed after 6 consecutive reuse cycles. Based on this material, a rapid and simple method for the determination of VMSs in water was developed using magnetic solid-phase extraction (MSPE) coupled with gas chromatography-mass spectrometry (GC-MS) analysis. The method enabled effective extraction of VMSs from water within 20 min, achieving recoveries ranging from 70.4% to 117.0%. The method limit of quantitation (LOQ) was 0.004 ng/mL, with intra-day precision (RSD) ranging from 0.9% to 3.9%. Analysis of real water samples revealed contamination in all 16 selected water bodies, with five specific VMSs species detected at concentrations ranging from 0.01 to 0.52 ng/mL. In summary, the proposed method enabled rapid and simple determination of VMSs in water samples, demonstrating significant potential for environmental analysis applications. Graphical abstract The alternative text for this image may have been generated using AI.