Abstract

A rapid, reliable and eco-friendly method for the determination of three sex hormones in five kinds of milk was developed and validated by combining vortex-assisted liquid-liquid microextraction (VALLME) and magnetic solid-phase extraction (MSPE). Deep eutectic solvents (DESs) such as choline chloride/urea were considered as the extraction solvent in VALLME and multi-walled carbon nanotubes (MMWCNTs) were used as the adsorbent which could adsorb DESs on the surface. The optimum experimental conditions were as follows: amount of MMWCNTs for 10 mg, volume of acetone for 4 mL, no sodium chloride and extraction pH at 7. After the optimization of several main variables, satisfactory sensitivity levels were achieved as low as 1.0–1.3 ng mL−1 and 2.5–4.5 ng mL−1 for the limit of method detections and the limit of method quantitation, respectively. The recoveries of the three hormones in different milk samples were in the range of 80.1%-116.4%. Consequently, this method is suitable for monitoring the trace amount of sex hormones in milk matrices.

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