Three-dimensional (3D) imprinting polymer based on graphene oxide-mesoporous silica nanobeads for chemometrics-assisted micro solid-phase extraction of lead in fish samples

• Published in: Journal of food composition and analysis 2024-04, Vol.128, p.106014, Article 106014
• Main Authors: Havasi, Tahere, Ezzatzadeh, Elham, Taheri, Alireza
• Format: Article
• Language: English
• Subjects: Adsorption; Fish sample; Pb(II); Surface imprinting; µ-solid phase extraction
• ISSN: 0889-1575; 1096-0481
• DOI: 10.1016/j.jfca.2024.106014

A rapid, sensitive, accurate and precise micro solid phase extraction method for the determination of Pb (II) in Fish sample by ionic imprinted polymer was developed on the surface of mesoporous silica and based on graphene oxide nanobeads. Extraction parameters were optimized using Box-Behnken design to achieve the twin objectives of quantitative determination and removal of Pb (II). Analytical figures of merit includes a linearity range of 0.01 to 250 µg L−1 (R2 = 0.9931), Limit of detection of 0.003 µg L−1 and Limit of quantification of 0.08 µg L−1. The maximum percentage of lead recovery (98.02% and desirability of 0.802) was obtained at pH 6.92, in 32.23 min contact time by 66.14 mg adsorbent. Accuracy was assessed by analysis of certified reference materials and the average percent recovery for the analytical methods were 99.35%. Recovery experiments after spiking in fish samples (salmon, sardines, yolks and tuna) was successfully carried out and high recoveries were 97.000–101.900% with low relative standard deviations of 0.022–0.016%. The optimal eluent condition was determined to be 25 μl of a 0.75 M solution of methanol-acetic acid. The maximum adsorption capacity, enrichment factor and repeatability was calculated as 16.67%, 89.5%, and 3.21% respectively, which shows the polymer selectivity for Pb2+ adsorption. Ease of use, rapid adsorption and high selectivity makes it a promising candidate for efficient and selective removal and trace determination. •A 3D Imprinting Polymer Based on GO-Mesoporous Silica Nanobeads was synthesized.•Micro solid phase extraction (µSPE) of trace amounts of Pb2+ has been proposed.•The behavior of variables was accurately modeled (BBD) and predicted.•Pb2+ was determined in fish samples using fast sequential-AAS (FS-AAS).