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Single Laboratory Validation – AOAC First Action Method 2012.22 Vitamin C in Infant Formula and Adult/Pediatric

Nutritional Formula by UPLC-UV

Date of Issue: February 14

th

, 2013

RDLS-RD130018

E.Campos Giménez (NRC/QS, Lausanne)

Page 8

Single Laboratory Validation,

Continued

Accuracy

studies

Reference material

: The overall mean of duplicate analysis of the certified

reference material SRM 1849a on 6 different days by 2 analysts was

70.3 mg/100 g, with a SD (standard deviation of the mean of duplicates) of 2.9

mg/100 g, which is not statistically different from the certified value (78.4 ± 6.5

g/100 g).

Spike recovery:

Results of spiking experiments are shown below. All recovery

rates complied with requirements (90-110 %).

Target +50 % of target + 100 % of target

Non fortified products

Avg

RSD

Avg

RSD

Child Formula Powder

4.4

111 % 0.9 %

98 %

1.8 %

Infant Elemental Powder

40

93 %

0.9 %

94 %

1.1 %

Adult Nutritional RTF High Prot

30

97 %

2.4 %

93 %

2.0 %

Adult nutritional RTF High Fat

35

98 %

1.1 %

95 %

2.3 %

Infant Formula RTF Milk Based

10

99 %

0.6 %

97 %

1.4 %

Example

chromatogra

ms

Ascorbic

AU

-0.005

0.000

0.005

0.010

0.015

0.020

0.025

0.030

0.035

0.040

0.045

0.050

Minutes

0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00

Ascorbic

AU

-0.005

0.000

0.005

0.010

0.015

0.020

0.025

0.030

0.035

0.040

0.045

0.050

Minutes

0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00

Ascorbic

AU

-0.005

0.000

0.005

0.010

0.015

0.020

0.025

0.030

0.035

0.040

0.045

0.050

Minutes

0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00

Ascorbic

AU

-0.005

0.000

0.005

0.010

0.015

0.020

0.025

0.030

0.035

0.040

0.045

0.050

Minutes

0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00

Standard solutionAscorbic acid2 µg/mL

Infant FormulaPowder Milk Based

Infant FormulaPowder Soy Based

SRM 1849a

Ascorbic

AU

0.00

0.02

0.04

0.06

0.08

0.10

0.12

0.14

0.16

0.18

0.20

Minutes

0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00

Ascorbic

AU

0.00

0.02

0.04

0.06

0.08

0.10

0.12

0.14

0.16

0.18

0.20

Minutes

0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00

Infant Elemental Powder

Adult Nutritional RTF HighFat

9 / 20

VitC-03/2012.22

For ERP Use Only

DO NOT DISTRIBUTE

AOAC OMB Meeting Book

318