P
oitevin
:
J
ournalof
AOAC I
nternational
V
ol
.
95, N
o
. 1, 2012
185
> 0.99995 for all recommended lines except for the potassium
line (R
2
= 0.99924).
LOQ
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 elementspresent at theseconcentrations (e.g.,Ca,Cu, Fe,K,
Na, andP in corn bran;Mg andZn in sterilized cream, andMn
in nonfatmilk powder).
Selectivity
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
60mg/L.
Recovery
Recovery values ranged between 79 and 120% for all
elements in allmatrixes for concentrations between0.26mg/kg
(Mn) and 16 900mg/kg (K).
Repeatability andReproducibility/Uncertainty
RSD
r
and RSD
iR
values for all elements in all matrixes
rangedbetween0.6 and16.9% and0.7 and23.3%, respectively,
for concentrations between0.26mg/kg (Mn) and16900mg/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 testedmatrixes.
Ruggedness
Recovery values for all elements in all matrixes ranged
between 67 and 118%. RSD
r
andRSD
iR
values for all elements
in all matrixes ranged between 0.4 and 18.9% and between 1
and73.6%, respectively, for concentrationsbetween0.26mg/kg
(Mn) and16900mg/kg (K).General applicabilityof themethod
is limited by less analytical experience and competency
regarding sample preparation (e.g., sample homogeneity and
adapted digestion program) and ICP analysis (adapted ion
buffering and use of robust conditions).
RingTrial Classical Statistics
The ring trial involved nine Nestlé laboratories that
volunteered to independently participate in the nutritional
elements studyoffivematrixes.This specificprocedureenabled
participants to independently and objectively analyze ring trial
samples, adding their contribution to the final validation of the
method.
See
Tables
2011.14A
–
I
.
Recovery
Recovery values ranged between 87 and 105% for all
elements in all matrixes for concentrations ranging between
0.4mg/kg (Mn) and 9700mg/kg (Ca).
Repeatability andReproducibility
RSD
r
and 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
9700mg/kg (K).
HorRat
HorRat values rangedbetween0.4 and1.2 for all elements in
allmatrixes for concentrations rangingbetween0.4mg/kg (Mn)
and 9700mg/kg (Ca).
Recommendations
From the data presented in this paper, the method is suitable
for detecting calcium, copper, iron, magnesium, manganese,
potassium,phosphorus,sodium,andzincinfortifiedfoodproducts
by microwave digestion and ICP-OES. It is recommended that
the method be adopted as an Official First Action Method of
AOAC INTERNATIONAL.
References
(1) Poitevin, E., Nicolas,M., Graveleau, L., Richoz, J.,Andrey, D.,
&Monard, F.
(2) Rousseew, P.,&Croux, C. (1993)
J. Am. Stat. Assoc.
88
,
1273–1283. doi.org/10.2307/2291267
MTE-01
FORWORKINGGROUP/ERPUSEONLY
DONOTDISTRIBUTE
