On-line Ultrasound-Assisted Dispersive Micro-Solid-Phase Extraction Based on Amino Bimodal Mesoporous Silica Nanoparticles for the Preconcentration and Determination of Cadmium in Human Biological Samples

• Published in: Biological trace element research 2016-06, Vol.171 (2), p.472-481
• Main Authors: Shirkhanloo, H, M. Falahnejad, H. Zavvar Mousavi
• Format: Article
• Language: English
• Subjects: Adsorption; atomic absorption spectrometry; Atomic absorption spectroscopy; Biochemistry; Biological samples; Biomedical and Life Sciences; Biotechnology; blood serum; Cadmium; Cadmium - blood; detection limit; Humans; Hydrogen-Ion Concentration; Internet; Ions; Life Sciences; Nanoparticles; Nanoparticles - chemistry; Nitric acid; Nutrition; nylon; Oncology; Particle Size; Porosity; porous media; Silica; Silicon Dioxide - chemistry; Solid Phase Extraction; Spectral analysis; Spectrometry; Spectrophotometry, Atomic; Surface Properties; Trace elements; Ultrasonic imaging; ultrasonic treatment; Ultrasonic Waves; ultrasonics
• ISSN: 0163-4984; 1559-0720
• DOI: 10.1007/s12011-015-0538-6

On-line ultrasound-assisted dispersive micro-solid-phase extraction (USA-DμSPE) has been developed for preconcentration and separation of trace amounts of Cd(II) ions in 0.5 mL of human biological samples. In a syringe with a nylon membrane, new synthetic bulky amino bimodal mesoporous silica nanoparticles (NH₂-UVM₇) were dispersed as a nanoadsorbent in 5 mL of diluted serum sample (1:10), and after ultrasonic shaking, the liquid phase was separated from the solid phase. At the optimized pH, the chemical and physical adsorption of cadmium ions occurred, respectively, based on complexation with amine groups of UVM₇ (Cd:NH₂-UVM₇) and silica nanoparticles. The analyte was then back-extracted from the sorbent with nitric acid solution (0.2 M), and its concentration was determined by electrothermal atomic absorption spectrometry (ETAAS). Under the optimized conditions, the linear range, limit of detection (LOD), and preconcentration factor (PF) were obtained as 0.01–0.56 μg L⁻¹, 0.002 μg L⁻¹, and 25, respectively. The adsorption capacity of NH₂-UVM₇ was found to be 108.6 mg g⁻¹ of cadmium. The validation of the methodology was performed by the human standard reference material (HSRM).