Magnetic nanoparticles grafted with β-cyclodextrin for solid-phase extraction of 5-hydroxy-3-indole acetic acid

• Published in: Mikrochimica acta (1966) 2014-07, Vol.181 (9-10), p.941-948
• Main Authors: Gaber Ahmed, Gaber Hashem, Badía Laíño, Rosana, García Calzón, Josefa Angela, Díaz García, Marta Elena
• Format: Article
• Language: English
• Subjects: Adsorbents; Analytical Chemistry; Cadmium; Characterization and Evaluation of Materials; Chemistry; Chemistry and Materials Science; Extraction; Fluorometers; Microengineering; Nanochemistry; Nanoparticles; Nanotechnology; Original Paper; Recovery; Solvents; Urine
• ISSN: 0026-3672; 1436-5073
• DOI: 10.1007/s00604-014-1192-y

We describe the synthesis of ß-cyclodextrin modified magnetic nanoparticles (CD-mNPs) as a material for solid-phase extraction of the cancer biomarker 5-hydroxy-indole-3-acetic acid (5-HIAA) from urine. The CD-mNPs were characterized by TEM, FTIR, and XRD, and the kinetics and adsorption isotherms were studied. The strong interaction between the CD-mNPs and 5-HIAA is the main driving force for recognition and extraction, while the magnetic core of the NPs allows their separation from the sample matrix. Recovery of 5-HIAA from the adsorbent using an adequate solvent regenerated the adsorbent for further use. 5-HIAA was then quantified by fluorometry of its complex with ß-CD. The method works in the 1 × 10 −7 to 1 × 10 −5  mol L −1 (R 2 0.9982–0.9996) concentration range, and the limits of detection (3σ) and quantification (10 σ) of the method are 1.2 × 10 −8  mol L −1 and 4.01 × 10 −8  mol L −1 5-HIAA, respectively. The recovery of 5-HIAA from urine samples spiked with 5-HIAA in three concentrations (1.4 × 10 −6 , 4.50 × 10 −6 and 1.0 × 10 −5  mol L −1 ) are within 63 ± 3 %. Figure Cyclodextrin functional magnetic nanoparticles as sorbents for separation of 5-hydroxy-3-indole acetic acid and its fluorescence determination after released with methanol.