AOAC SPIFAN Stakeholder Panel Meeting Book (September 7, 2019)

AOAC SMPR 2011.004

Applicability Determination of total vitamin D 2

and vitamin D 3 in all forms (powders, ready-to-feed liquids, and liquid concentrates) of infant, adult, and pediatric nutritional formulas. For the purpose of this SMPR, vitamin D 2 is defined as ergocalciferol (CAS 8017-28-5) and its previtamin isomer; and vitamin D 3 is defined as cholecalciferol (CAS 67-97-0) and its previtamin isomer. Criteria Value Analytical Range 0.12–5.1 μg/100g b Limit of Detection ” —J J b Limit of Quantitation ” —J J b

” ”

0.12–1.5 μg/100g b

Repeatability (RSD r )

>1.5 μg/100g b

80– 90–

0.12–1.5 μg/100g b

Recovery

>1.5 μg/100g b

Reproducibility (RSD R ) ” a Concentrations apply to (1) “ready-to-feed” liquids “as is”; (2) reconstituted powders (25 g into 200 mL water); and (3) liquid concentrates diluted 1:1 by weight. b μg/100 g expressed separately as vitamin D 2 and vitamin D 3 in reconstituted final product.

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133 rd Annual Meeting & Exposition | Denver, Colorado | September 6-12, 2019

AOAC 2016.05 Performance

Method Performance As part of MLT validation phase, AOAC Official Method 2016.05 was evaluated against the SMPR in 9-laboratories using 9 different infant formula products.

Precision parameters

A

B

C

E

G I

M O P

Number of labs

9

9

9

9

9

9

9

9

9

Number of replicates Number of outliers

36

18

18

18

18

18

18

18

18

0

0

0

0

0

0

0

0

0

Grand mean

10.2

8.6 0.3 0.8 3.9

8.2 0.2 0.7 2.3

9.9 0.4 1.1 4.2

8.3 0.4 0.6 4.3

0.7 0.0 0.1 3.6

8.8 0.3 0.6 3.2

10.1

6.9 0.3 0.6 4.9

Repeatability SD Reproducibility SD Repeatability RSD Repeatability limit Reproducibility RSD Reproducibility limit

0.3 0.7 3.2

0.5 0.8 5.1

11.0

11.0

11.0

11.0 10.9 15.0

11.0

11.0 11.4 15.0

11.0

11.0

11.0

7.2

8.8

8.2

7.7

6.4

8.3

9.1

15.0

15.0

15.0

15.0

15.0

15.0

15.0

Horwitz ratio

0.3 0.4 A = NIST SRM1849a, B = partially hydrolyzed soy-based infant formula powder, C = infant elemental powder, E = soy-based infant formula, G = infant formula powder, I = milk-based infant formula ready-to- feed, M = partially hydrolyzed milk-based infant formula powder, O = milk-based infant formula, P = fructoligosaccharide, galactooligosaccharide-based infant formula powder 0.4 0.3 0.5 0.3 0.3 0.3 0.4

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133 rd Annual Meeting & Exposition | Denver, Colorado | September 6-12, 2019