AOAC SPIFAN Review Team (August 2016)

Dual Lab Validation of a Method for the Determination of Fructans in Infant

Formula & Adult Nutritionals /

25 Jul 2016

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

, 2016

May 23

, 2016

Fructan

(%m/m)

Meet

requirements

Fructan (%m/m)

Meet

requirements

0.044

0.048

0.002

0.003

LOD = 3 x SD

0.005

Yes

0.009

Yes

LOQ = 10 x SD

0.016

yes

0.030

yes

In which:

= individual result of the measured fructan content in the spiked sample

= average fructan content

= 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 %.

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

VALIDATION REPORT

FOR ERP USE ONLY

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