Dual Lab Validation of a Method for the Determination of Fructans in Infant
Formula & Adult Nutritionals /
25 Jul 2016
41
Table 4
Summarizing results of the LOD and LOQ determination in the
reconstituted sample no 7, Infant formula powder partially hydrolyzed
milk based.
February 28
th
, 2016
May 23
rd
, 2016
Fructan
(%m/m)
Meet
requirements
Fructan (%m/m)
Meet
requirements
0.044
0.048
SD
r
0.002
0.003
LOD = 3 x SD
0.005
Yes
0.009
Yes
LOQ = 10 x SD
r
0.016
yes
0.030
yes
In which:
x
i
= individual result of the measured fructan content in the spiked sample
= average fructan content
SD
r
= repeatability standard deviation in the average fructan content
Moreover these data can also be applied to calculate the average recovery of the spiked amounts
fructan in both series. The fructan addition was 0.046 % and the average fructan content in the tenfold
analyses was 0.044 (Febr. 28) respectively 0.048 % (May 23), corresponding with average recoveries of
95.6 and 104.3% of the added amount fructan. This is very well within the target range of 90 – 110 %.
d.
Precision
Based on the analytical results reported in table 2, 6 of the 7 fructan containing not‐reconstituted
samples (marked in yellow in table 2) are selected for this precision study. Sample 8 was excluded. The
fructan content in the reconstituted sample 8 will be less than the LOQ. And after spiking this sample
with 50% and 150% of its original fructan content, the spiked fructan content is still less than the LOQ
meaning that this experiment will not result in reliable data.
The analyses for this precision study have been done at six different days in the period March – June
2016 by 2 different technicians and applying three different HPAEC‐PAD instrument (one ICS3000
instrument and two different ICS5000 instruments) and each instrument was equipped with its own
chromatographic column (Carbopack PA‐1).
The results of the precision study are summarized in table 5. All experimental results of this precision
study are given in Annex D
x
x
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