AOAC OMA# 2011.14 (Final Action Review)-OMB

2011.14 (MTE-01) MLT FOR ERP USE ONLY DO NOT DISTRIBUTE

P oitevin : J ournal of AOAC I nternational V ol . 95, N o . 1, 2012  185

adapted digestion program) and ICP analysis (adapted ion buffering and use of robust conditions).

> 0.99995 for all recommended lines except for the potassium line (R 2 = 0.99924).

Ring Trial Classical Statistics

LOQ

The ring trial involved nine Nestlé laboratories that volunteered to independently participate in the nutritional elements study of five matrixes. This specific procedure enabled participants to independently and objectively analyze ring trial samples, adding their contribution to the final validation of the method. See Tables 2011.14A – I .

The LOQ of elements (mg/kg): Ca (150); Cu (2); Fe (10); K (200); Mg (50); Mn (0.05); Na (100); P (100); and Zn (5) were estimated in real matrixes with satisfactory recovery, repeatability RSD r , and reproducibility RSD iR values obtained for elements present at these concentrations (e.g., Ca, Cu, Fe, K, Na, and P in corn bran; Mg and Zn in sterilized cream, and Mn in nonfat milk powder).

Recovery

Selectivity

Recovery values ranged between 87 and 105% for all elements in all matrixes for concentrations ranging between 0.4 mg/kg (Mn) and 9700 mg/kg (Ca).

Recovery values ranged between 88 and 115% in all spiked food-grade salt solutions with SDs between 0.1 and 18.8% for spiking with element of interest that ranged between 0.01 and 60 mg/L.

Repeatability and Reproducibility

RSD r values for all elements in all matrixes ranged between 1.0 and 6.8% and between 1.9 and 12.5%, respectively, for concentrations between 0.4 mg/kg (Mn) and 9700 mg/kg (K). and RSD R

Recovery

Recovery values ranged between 79 and 120% for all elements in all matrixes for concentrations between 0.26 mg/kg (Mn) and 16 900 mg/kg (K).

HorRat

Repeatability and Reproducibility/Uncertainty

HorRat values ranged between 0.4 and 1.2 for all elements in all matrixes for concentrations ranging between 0.4 mg/kg (Mn) and 9700 mg/kg (Ca).

RSD r values for all elements in all matrixes ranged between 0.6 and 16.9% and 0.7 and 23.3%, respectively, for concentrations between 0.26 mg/kg (Mn) and 16 900 mg/kg (K). Calculated derived relative uncertainty (U) values for all elements in all tested matrixes ranged from 1 to 26% for all elements in the seven tested matrixes. and RSD iR

Recommendations

From the data presented in this paper, the method is suitable for detecting calcium, copper, iron, magnesium, manganese, potassium, phosphorus, sodium, and zinc in fortified food products by microwave digestion and ICP-OES. It is recommended that the method be adopted as an Official First Action Method of AOAC INTERNATIONAL.

Ruggedness

Recovery values for all elements in all matrixes ranged between 67 and 118%. RSD r and RSD iR values for all elements in all matrixes ranged between 0.4 and 18.9% and between 1 and 73.6%, respectively, for concentrations between 0.26 mg/kg (Mn) and 16900 mg/kg (K). General applicability of the method is limited by less analytical experience and competency regarding sample preparation (e.g., sample homogeneity and

References

 (1) Poitevin, E., Nicolas, M., Graveleau, L., Richoz, J., Andrey, D., & Monard, F. (2009) J. AOAC Int. 92 , 1484–1518  (2) Rousseew, P., & Croux, C. (1993) J. Am. Stat. Assoc. 88 , 1273–1283. doi.org/10.2307/2291267