<p>A novel magnetic nanocomposite, ZIF-67-functionalized magnetic multi-walled carbon nanotubes (MMWCNT@ZIF-67), was successfully synthesized and applied as an adsorbent for the magnetic solid-phase extraction (MSPE) of benzodiazepines (BDZs) from water samples. Comprehensive characterization by FT-IR, XRD, VSM, XPS, SEM and TEM confirmed the successful anchoring of Fe₃O₄ nanoparticles onto the carbon nanotube surface and the in-situ growth of ZIF-67 crystals, forming a core–shell structured composite. The material exhibited favorable magnetic properties for rapid separation and a microporous structure. Adsorption performance studies demonstrated that MMWCNT@ZIF-67 exhibited excellent adsorption capacity for diazepam (DZP), with a maximum adsorption capacity of 459.42&#xa0;mg/g. The simulation results of the adsorption isotherms and adsorption kinetics indicate that the adsorption behavior of the composite material involves physic and chemical process. Based on this material, an MSPE method coupled with high-performance liquid chromatography equipped with either a variable wavelength detector (HPLC-VWD) or tandem mass spectrometry (HPLC-MS/MS) was optimized and established. Method validation showed high sensitivity (limits of detection of 0.0009–0.004 ng/mL for HPLC-MS/MS), good accuracy (spiked recoveries of 87.5–101.3%), and satisfactory reusability of the adsorbent over five consecutive cycles with consistent performance. This work provides an efficient, green, and reliable analytical approach for monitoring trace-level psychoactive pharmaceuticals in environmental water samples.</p> Graphical Abstract <p></p>

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ZIF-67 functionalized magnetic multi-walled carbon nanotubes for magnetic solid-phase extraction of benzodiazepines in water samples

  • Hong-Liang Xiao,
  • Ting-Ting Li,
  • Si-Ting Li,
  • Shuang-Cheng Bai,
  • Lu Han,
  • Lin Xin,
  • Xiao-Ping Liao,
  • Dong-Hao Zhao

摘要

A novel magnetic nanocomposite, ZIF-67-functionalized magnetic multi-walled carbon nanotubes (MMWCNT@ZIF-67), was successfully synthesized and applied as an adsorbent for the magnetic solid-phase extraction (MSPE) of benzodiazepines (BDZs) from water samples. Comprehensive characterization by FT-IR, XRD, VSM, XPS, SEM and TEM confirmed the successful anchoring of Fe₃O₄ nanoparticles onto the carbon nanotube surface and the in-situ growth of ZIF-67 crystals, forming a core–shell structured composite. The material exhibited favorable magnetic properties for rapid separation and a microporous structure. Adsorption performance studies demonstrated that MMWCNT@ZIF-67 exhibited excellent adsorption capacity for diazepam (DZP), with a maximum adsorption capacity of 459.42 mg/g. The simulation results of the adsorption isotherms and adsorption kinetics indicate that the adsorption behavior of the composite material involves physic and chemical process. Based on this material, an MSPE method coupled with high-performance liquid chromatography equipped with either a variable wavelength detector (HPLC-VWD) or tandem mass spectrometry (HPLC-MS/MS) was optimized and established. Method validation showed high sensitivity (limits of detection of 0.0009–0.004 ng/mL for HPLC-MS/MS), good accuracy (spiked recoveries of 87.5–101.3%), and satisfactory reusability of the adsorbent over five consecutive cycles with consistent performance. This work provides an efficient, green, and reliable analytical approach for monitoring trace-level psychoactive pharmaceuticals in environmental water samples.

Graphical Abstract