Simultaneous determination of four sedative- hypnotics in human urine based on dendritic structured magnetic nanomaterials

A magnetic solid-phase extraction technique based on magnetic dendritic structured nanoparticles (Fe3O4@SiO2-NH2-G5) as adsorbent coupled with ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) has been developed to detect diaze-pam, midazolam, zolpidem, and zaleplon in human urine. With Fe3O4@SiO2-NH2 as the central core, dendrimer (G5) grafted alternately with cyanuric chloride and imidazole were bonded to the surface of the core to synthesize Fe3O4@SiO2-NH2-G5. The morphology and structure of the magnetic materials were characterized by transmission electron microscopy (TEM), Fourier trans-form infrared spectroscopy (FT-IR), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), and dynamic light scattering (DLS). The key parameters affecting the extraction efficiency were optimized. A satisfactory performance was obtained under the optimum extraction conditions. The proposed method was validated, and the limits of detection of zaleplon, diazepam, zolpidem, and midazolam were 0.05, 0.05, 0.02, and 0.02 ng mL-1, respectively. The linear correlation coef-ficients r of the four analytes were > 0.996, the intra-day precision was between 2.4 % and 9.4 % with the recoveries between 88.3 % and 104.8 %, and the inter-day precision ranged from 3.9 % to 15.2 % with the recovery in the range of 94.1 %-108.3 %. The magnetic dendritic structure nano -material Fe3O4@SiO2-NH2-G5 was successfully used to extract sedative-hypnotic drugs from human urine samples. The Fe3O4@SiO2-NH2-G5-based magnetic solid-phase extraction method eliminates centrifugation and filtration steps as in conventional extraction. Only one step of vortex dispersion extraction could achieve the separation and purification of the target compounds. The proposed method was simple, rapid, environment-friendly, and suitable for the analysis of sedative-hypnotic drugs in human urine.(c) 2022 The Author(s). Published by Elsevier B.V. on behalf of King Saud University. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

Automated summary

A magnetic solid-phase extraction technique based on magnetic dendritic structured nanoparticles coupled with ultra-high performance liquid chromatography tandem mass spectrometry was developed for the detection of sedative-hypnotic drugs in human urine. The method was simple, rapid, and achieved satisfactory separation and purification.