Use of fractional factorial design for optimization of digestion procedures followed by multi-element determination of essential and non-essential elements in nuts using ICP-OES technique.

Two digestion procedures have been tested on nut samples for application in the determination of essential (Cr, Cu, Fe, Mg, Mn, Zn) and non-essential (Al, Ba, Cd, Pb) elements by inductively coupled plasma-optical emission spectrometry (ICP-OES). These included wet digestions with HNO(3)/H(2)SO(4) and HNO(3)/H(2)SO(4)/H(2)O(2). The later one is recommended for better analytes recoveries (relative error<11%). Two calibrations (aqueous standard and standard addition) procedures were studied and proved that standard addition was preferable for all analytes. Experimental designs for seven factors (HNO(3), H(2)SO(4) and H(2)O(2) volumes, digestion time, pre-digestion time, temperature of the hot plate and sample weight) were used for optimization of sample digestion procedures. For this purpose Plackett-Burman fractional factorial design, which involve eight experiments was adopted. The factors HNO(3) and H(2)O(2) volume, and the digestion time were found to be the most important parameters. The instrumental conditions were also optimized (using peanut matrix rather than aqueous standard solutions) considering radio-frequency (rf) incident power, nebulizer argon gas flow rate and sample uptake flow rate. The analytical performance, such as limits of detection (LOD<0.74mugg(-1)), precision of the overall procedures (relative standard deviation between 2.0 and 8.2%) and accuracy (relative errors between 0.4 and 11%) were assessed statistically to evaluate the developed analytical procedures. The good agreement between measured and certified values for all analytes (relative error <11%) with respect to IAEA-331 (spinach leaves) and IAEA-359 (cabbage) indicates that the developed analytical method is well suited for further studies on the fate of major elements in nuts and possibly similar matrices.