Dispersive Micro-Solid Phase Extraction Using a Graphene Oxide Nanosheet with Neocuproine and Batocuproine for the Preconcentration of Traces of Metal Ions in Food Samples

A dispersive micro-solid phase extraction (D mu-SPE) method for the preconcentration of trace metal ions (Pb, Cd, Cr, Mn, Fe, Co, Ni, Cu, Zn) on graphene oxide with the complexing reagents neocuproine or batocuproine is presented here. Metal ions form cationic complexes with neocuproine and batocuproine. These compounds are adsorbed on the GO surface via electrostatic interactions. The factors affecting the separation and preconcentration of analytes such as pH, eluent (concentration, type, volume), amount of neocuproine, batocuproine and GO, mixing time, and sample volume were optimized. The optimal sorption pH was 8. The adsorbed ions were effectively eluted with 5 mL 0.5 mol L-1 HNO3 solution and determined by the ICP-OES technique. The preconcentration factor for the GO/neocuproine and GO/batocuproine in the range 10-100 and 40-200 was obtained for the analytes, with detection limits of 0.035-0.84 ng mL (-1) and 0.047-0.54 ng mL(-1), respectively. The method was validated by the analysis of the three certified reference materials: M-3 HerTis, M-4 CormTis, and M-5 CodTis. The procedure was applied to determine metal levels in food samples.

Automated summary

A method of dispersive micro-solid phase extraction (D mu-SPE) using graphene oxide and complexing reagents neocuproine or batocuproine is presented for the preconcentration of trace metal ions (Pb, Cd, Cr, Mn, Fe, Co, Ni, Cu, Zn). The metal ions form cationic complexes and are adsorbed on the graphene oxide surface. Various factors such as pH, eluent, neocuproine and batocuproine amount, mixing time, and sample volume were optimized. The method was validated and applied for metal level determination in food samples.