AOAC SPIFAN Nutrients ERP (December 7, 2022)

For ERP/Working Group Use Only DO NOT DISTRIBUTE Fluor-04 (SLV) Resubmission FOR ERP USE ONLY DO NOT DISTRIBUTE

complex any free calcium or other polyvalent cations. The validation samples were tested by multiple analysts over multiple days. The same samples were sent to a third-party testing lab and were analyzed there using AOAC method 944.08 for analysis of fluoride in food. This method involved an alkaline ash procedure, followed by steam distillation from perchloric acid, and the subsequent titration of fluoride with thorium nitrate. All samples with fluoride concentrations < 0.5 ppm agreed with the TPL results within ± 1 ppm, and the samples with > 0.5 ppm fluoride agreed within ± 15%. Within day precision was < 8%, and the overall precision was < 10%. All validation criteria were met. The current method was submitted previously to the SPIFAN ERP for consideration (Fluor-04). The results presented did not agree with results collected by another technique (ion chromatography), so neither method was recommended for First Action. Both study directors were asked to resubmit if desired. In the interim, an additional 2 method SLVs were presented. These methods tested the same five samples analyzed in the current SLV. Their data are presented alongside the data from this method in Table XIII . Current results are shown in units of “ µg F/100g reconstitution” (SMPR requested units) and “µg F/g powder”. The latter results compare well with results from the other methods, especially those from Fluor-06. The samples that tested below the LOD (8260 and Infant formula C) show the greatest difference between methods.

Table IIIIII: Comparison of results from multiple methods

Current method average (µg F/100g reconstitution)

Current method average (µg F/g powder)

Fluor-05 ‘amount on powder (µg/100g)’

Fluor-06 ‘(µg/100g)’

Sample

Infant formula A

16.33 14.81

147.0 133.3

96.0 94.1 20.7 59.0 34.7

148.5 126.4

1869 8260 8261

3.48

31.4 92.5 42.7

19.1 97.5 34.0

10.28

Infant formula C

4.74

Funding : This research was conducted without any outside funding sources Conflict of Interest : The authors declare there are no conflicts of interest.

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