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12

H

ostetler

:

J

ournal of

AOAC I

nternational

V

ol

.

100, N

o

.

3, 2017

accuracy was assessed by spike and recovery of all-

trans

-lutein

and β-carotene in various matrixes. Spiking was done with

either FloraGlo 5% lutein (DSM Nutritional Products, Basel,

Switzerland), which was first dispersed in water and added

to the sample in place of water, or with diluted standards

added to the ISTD. Spiked and unspiked samples were

measured in triplicate. Tables 11–17 show that recovery from

spiked samples ranged from 92.3 to 105.5% for lutein and

from 100.1 to 107.5% for β-carotene. The SMPR calls for

90–110% recovery from spiked samples, and all data met this

requirement.

Conclusions

The data presented here were reviewed by the AOAC

Expert Review Panel on SPIFAN Nutrient Methods at the AOAC

INTERNATIONAL Annual Meeting in Dallas, TX, held in

September 2016. The panel found that the data met the criteria

Table 10. Precision data for β-carotene in SPIFAN matrixes and select additional matrixes

a

Formula

Code

n

cis

-BC,

μg/100 g

b

RSD

r

, % RSD

iR

, %

trans

-BC,

μg/100 g RSD

r

, % RSD

iR

, %

Total BC,

μg/100 g RSD

r

, % RSD

iR

, %

Child Formula Powder,

Placebo

00847RF00 3

0.3

0.7

NA

c

0.6

2.6

NA 0.9

1.8

NA

Infant Elemental Powder,

Placebo

00796RF 3

<

d

NA

NA

<

NA NA

<

NA NA

AN High-Protein RTF,

Placebo

e

00821RF00 3

<

NA

NA

0.8

11.2

NA 0.8

11.2

NA

AN High-Fat RTF, Placebo 00820RF00 3

<

NA

NA

0.4

47.4

NA 0.6

48.5

NA

IF Milk-Based RTF, Placebo

f

EV4H2Q 3

0.5

3.3

NA

0.4

2.2

NA 0.9

2.6

NA

SRM 1849a Powder

CLC10-B 3

<

NA

NA

<

NA NA

<

NA NA

IF Milk-Based Partially

Hydrolyzed Powder

410057652Z 3

0.8

0.2

NA

1.0

2.0

NA 1.8

1.2

NA

IF Soy-Based Partially

Hydrolyzed Powder

410057651Z 3

0.6

1.8

NA

0.6

6.7

NA 1.3

3.9

NA

Toddler Formula

Milk-Based Powder

4052755861 12

6.5

1.0

2.4

7.4

0.7

2.9

13.9

0.8

2.2

IF Milk-Based Powder

4044755861 12

4.4

2.1

2.7

10.1

1.3

2.7

14.4

1.5

2.4

AN Powder

00859RF00 3

<

NA

NA

0.3

5.9

NA 0.3

5.9

NA

Child Formula Powder

00866RF00 3

0.3

15.3

NA

0.4

2.5

NA 0.7

5.4

NA

IF Elemental Powder

00795RF 12

7.3

0.3

0.7

15.3

0.7

0.7

22.7

0.5

0.6

IF with FOS/GOS Powder

g

50350017W1 12

1.3

5.1

6.3

3.4

3.0

4.6

4.8

2.3

3.8

IF Milk-Based Powder

(control)

K16NTAV 39

6.0

1.1

2.7

13.2

0.5

2.2

19.2

0.6

1.7

IF Soy-Based Powder

E10NWZC 12

6.5

2.6

2.3

11.0

2.0

1.8

17.5

2.2

1.9

IF Milk-Based RTF

EV4H2R 3

0.6

6.9

NA

0.4

4.8

NA 1.0

4.6

NA

AN High-Protein RTF

00730RF00 12 265

1.6

2.7

534

1.7

2.3

799

1.6

2.4

AN High-Fat RTF

00729RF00 3

<

NA

NA

0.3

7.7

NA 0.4

5.9

NA

AN High-Lutein Powder

h

3

<

NA

NA

0.5

18.3

NA 0.5

18.3

NA

Chocolate Pediatric

Nutritional RTF

— 3

<

NA

NA

<

NA NA

<

NA NA

IF RTF

— 3

9.1

0.3

NA

16.4

0.4

NA 25.5

0.4

NA

a

 For powder samples, results were calculated using a factor of 25 g powder/225 g reconstituted weight.

b

 BC = β-Carotene.

c

 NA = Not applicable. RSDr not calculated for concentrations <LOQ; RSDiR not calculated if samples were all prepared on the same day.

d

 < = Below the LOQ.

e

 AN = Adult Nutritional.

f

 IF = Infant Formula.

g

 FOS/GOS = Fructooligosaccharide/galactooligosaccharide.

h

 — = Sample was sourced locally and was not part of the SPIFAN kit.

Table 11. Spike and recovery data for NIST SRM 1849a

a

Analyte

Native level, μg/100 g

Spike, μg/100 g Recovery, % RSD, % Spike, μg/100 g Recovery, % RSD, %

Lutein

ND

b

1.4

105.5

0.8

13.8

99.6

0.2

β-Carotene

0.2

1.3

107.5

0.9

13.6

103.2

0.3

a

 Samples were spiked with standards at the internal standard step of sample preparation.

b

 ND = Not detected.

52