Development and optimization of a vortex-assisted micro-solid phase extraction (VA-µSPE) method for sensitive fluoxetine determination using a novel CoNiCr-LDH@ND-COOH nanocomposite


Özen M. B., Hassan Ahmed H. E., SALAMAT Q., SOYLAK M.

Analytical Methods, 2026 (SCI-Expanded, Scopus)

  • Yayın Türü: Makale / Tam Makale
  • Basım Tarihi: 2026
  • Doi Numarası: 10.1039/d6ay01402j
  • Dergi Adı: Analytical Methods
  • Derginin Tarandığı İndeksler: Science Citation Index Expanded (SCI-EXPANDED), Scopus, Compendex, EMBASE, MEDLINE
  • Erciyes Üniversitesi Adresli: Evet

Özet

In this work, an innovative CoNiCr-LDH@ND-COOH nanocomposite was synthesized and utilized as an efficient adsorbent for the effective extraction of fluoxetine. The nanocomposite structure combines the exceptional adsorption performance and capacity of carboxyl-functionalized nanodiamonds with the large surface area and tunable chemistry of layered double hydroxides (LDHs). The synthesized materials were characterized using FESEM, FESEM-EDX, FTIR, XRD, and BET analyses. These analyses demonstrated the nanocomposite’s structural strength and surface characteristics. The developed extraction method was designed and optimized using Plackett–Burman and Central Composite Design methods. The optimal extraction conditions were as follows: 30 mg of adsorbent, pH 6.5, adsorption/desorption times of 5 minutes, ethanol as the eluent, and centrifugation at 4100 rpm. The method exhibited excellent analytical performance, with recoveries ranging from 87 to 99% at 225 nm (HPLC-DAD), a preconcentration factor of 50, a linear range of 1 to 5000 µg L−1, a LOD of 0.25 µg L−1, and a LOQ of 0.75 µg L−1. The precision was acceptable, with intra- and inter-day RSD values of 4.8% and 6.7%, respectively. Furthermore, the adsorbent showed acceptable reusability for eight cycles. The presented method is robust, sensitive, and reusable for the extraction and determination of fluoxetine.