Multivariate Optimization of a Green Microwave-Assisted Hydrogen Peroxide Digestion of Vegetable Oils and Subsequent Elemental Determination Via Inductively Coupled Plasma–Optical Emission Spectrometry

A microwave-assisted digestion technique based on dilute hydrogen peroxide (MW-AHPD) was developed for multielemental determination in vegetable oils. The determination of ten trace elements (As, Cd, Cr, Cu, Fe, Pb, Ni, Sn, V, and Zn) was conducted via inductively coupled plasma optical emission spectroscopy (ICP-OES) after digestion. The most influential parameters were investigated by using multivariate optimization tools (two-level full factorial and central composite design) with percent recovery as the chemometric response. The optimum conditions were 2.0 mol L⁻¹ (H₂O₂]), 156 °C (digestion temperature),  0.1 g (sample mass) and 50 min (digestion time). Under the optimized conditions, the efficiency of digestion was evaluated based on the residual carbon content (RCC) of the final digests. The RCC values were very low, ranging from 0.84 to 1.60% (m/m). The greenness of the technique was evaluated using the Analytical Eco-scale, and the proposed method was considered an excellent green analysis method with a final score of 90. The accuracy of the optimized MW-AHPD was evaluated by spiking sunflower, olive, and peanut oils at concentrations of 2.5 and 5.0 μg L⁻¹, and excellent recoveries between 90.3 and 107.3% were reported. The accuracy of the MW-AHPD method was compared with that of microwave-assisted digestion using concentrated HNO₃, and there was no significant difference between the two methods. The limits of detection ranged from 0.026 to 14.6 μg L⁻¹. On the other hand, the interday and intraday precisions were less than 6.67 and 6.96%, respectively. The method was successfully applied to determine the concentrations of trace elements in 5 vegetable oils on the South African market. Thus, MW-AHPD-ICP–OES is applicable for the determination of trace elements in vegetable oils.