Microwave-assisted digestion method using diluted nitric acid and hydrogen peroxide for the determination of major and minor elements in milk samples by ICP-OES and ICP-MS

Abstract

A novel method for microwave-assisted digestion of milk samples using diluted HNO3and H2O2 with a single reaction chamber was developed for elemental analysis by ICP-based techniques. The optimal conditions for digestion were 0.25 g of sample mass, 6 mL of 0.1 molL−1HNO3and 2 mL of 30% H2O2 at 250 ℃ and 160 bar. The optimized procedure resulted in low residual carbon content and residual acidity of 260 mgL−1 and 0.06 mol L−1, respectively. The limits of detection ranged from 0.286ոg g−1(Ca) to 82.990ոg g−1(Fe). In addition, the proposed method was considered an excellent green analysis method with a final score of 87 based on the analytical Eco-Scale. Finally, the method was validated and applied to the determination of Al, As, Ba, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Sb, Se, and Zn in milk samples from South Korea.