A novel NiCoFe LDH/B-CDs-coated falcon tube for vortex assisted micro solid phase extraction of Cd (II) from food and water samples prior to its quantification by using a HR-CS-FAAS

Ahmed H. E. H., SALAMAT Q., SOYLAK M.

Microchemical Journal, cilt.225, 2026 (SCI-Expanded, Scopus) identifier identifier

  • Yayın Türü: Makale / Tam Makale
  • Cilt numarası: 225
  • Basım Tarihi: 2026
  • Doi Numarası: 10.1016/j.microc.2026.118112
  • Dergi Adı: Microchemical Journal
  • Derginin Tarandığı İndeksler: Science Citation Index Expanded (SCI-EXPANDED), Scopus, BIOSIS, Chemical Abstracts Core, Chimica, Index Islamicus
  • Anahtar Kelimeler: B-doped carbon dots, Cadmium, Fixed-bed extraction tube, NiCoFe layered double hydroxide, Vortex-assisted µSPE
  • Erciyes Üniversitesi Adresli: Evet

Özet

In this study, a coated Falcon tube vortex-assisted micro-solid phase extraction (CFT-VA-μSPE) method was developed for trace determination of Cd(II), employing a flower-like B-CDs@NiCoFe-LDH nanocomposite immobilized on the inner surface of a Falcon tube. The nanocomposite, synthesized via a two-step hydrothermal route using boron-doped carbon dots and NiCoFe LDH, featured a large surface area, abundant functional groups, and synergistic active sites conducive to Cd(II) adsorption. This fixed-bed configuration enabled direct adsorption-desorption without the need for post-extraction centrifugation or phase separation, substantially reducing solvent use and allowing for material reusability. Under optimized conditions (pH 8.0; 3 min adsorption; 5 min desorption; 2 mL of 2 mol L−1 HNO3), the method delivered excellent analytical performance, achieving an LOD of 1.73 μg L−1, LOQ of 5.77 μg L−1, preconcentration factor of 22.5, enhancement factor of 20.1, and RSD of 4.6%. Validation using certified reference materials (NCS ZC73032 Celery and BCR 505 Estuarine Water) and application to 15 real samples, including juices, soft drinks, natural waters, and wastewater, confirmed the method's reliability in the investigated matrices and generally good tolerance toward common coexisting ions. This work introduces a relatively green and reusable VA-μSPE platform that provides satisfactory analytical performance for Cd(II) monitoring in food and water samples. Its strong analytical capability and favorable green chemistry assessment (AGREE: 0.66; AGREEprep: 0.55; ComplexMoGAPI: 83.0; and White Analytical Chemistry: 83.0) position it as a promising benchmark for future sample preparation and metal-pollution surveillance.