This study focuses on the optimization of key operational parameters in dispersive magnetic solid phase microextraction (d-MSPE) using a response surface methodology based on the Box-Behnken design (BBD-RSM). The aim was to enhance the efficiency and accuracy of preconcentration and determination of lead(II), copper(II), and cadmium(II) ions in shellfish samples. A novel nanocomposite, ionic liquid-coated amino silanized magnetic graphene oxide (MGO@SiO2-APTES-IL), served as the adsorbent, combining magnetic separation capability with high surface functionalization for effective metal ion capture. Three critical variables—solution pH, adsorbent dosage, and extraction time—were evaluated during the adsorption step, while eluent concentration, elution volume, and desorption time were optimized during the desorption phase. Each factor was tested at three levels, resulting in 17 experimental runs designed to model quadratic relationships between variables and responses.
The statistical analysis revealed that all selected factors significantly influenced recovery rates, with interaction effects clearly observed in response surface plots. For the adsorption step, optimal performance was achieved at a pH of 5.6, an adsorbent dosage of 25.6 mg, and an extraction time of 6.3 minutes. At this pH, the surface charge of the nanocomposite favored electrostatic attraction of cationic metal ions, while avoiding hydroxide precipitation at higher pH values. Increasing the adsorbent amount enhanced active site availability, but excessive amounts led to aggregation and reduced efficiency. Similarly, longer extraction times improved contact equilibrium, yet beyond 6.3 minutes, no significant improvement was observed, indicating saturation of binding sites.
For the elution step, the best results were obtained with a 7.0% (v/v) nitric acid solution, a volume of 3.AQP1 Antibody Purity & Documentation 1 mL, and a desorption time of 6.6 minutes. Higher acid concentrations increased proton competition, facilitating complete desorption of metal ions from the sorbent surface. However, excess volume diluted the analytes, reducing final concentration. The optimized conditions enabled near-complete recovery (>93%) of target ions across all metals.CD35 Antibody Cancer The quadratic models derived from BBD-RSM exhibited high determination coefficients (R² = 0.PMID:35067601 9915 and adjusted R² = 0.9807), confirming strong predictive power and model adequacy. Lack-of-fit tests further validated the model’s reliability.
These findings demonstrate that BBD-RSM is a powerful tool for systematically optimizing complex analytical procedures involving multiple interacting variables. By identifying the ideal balance among parameters, the method ensures maximum sensitivity and reproducibility without extensive trial-and-error experimentation. This approach not only improves the precision of d-MSPE but also reduces reagent consumption and sample processing time. The optimized protocol enables rapid, accurate, and environmentally friendly analysis of trace metals in shellfish, supporting compliance with regulatory limits and enhancing food safety assessments. Moreover, the methodology can be readily adapted to other matrices or target analytes, offering broad applicability in environmental and biomedical research. The integration of advanced statistical modeling with innovative nanomaterial-based extraction techniques represents a significant advancement in modern analytical chemistry.MedChemExpress (MCE) offers a wide range of high-quality research chemicals and biochemicals (novel life-science reagents, reference compounds and natural compounds) for scientific use. We have professionally experienced and friendly staff to meet your needs. We are a competent and trustworthy partner for your research and scientific projects.Related websites: https://www.medchemexpress.com
