AOAC SPIFAN Nutrients ERP-Final Review (Jan. 2019)

Chol-08/Carn-07 (February 2016) FOR ERP USE ONLY DO NOT DISTRIBUTE

Table 11. LOQ Total Analysis

Choline Day/

Fortification (mg/100g)

Innate

Marginal Recovery

MEAN

SD (%) 1.2

RSD r

Replicate

(mg/100g)

(%)

(%)

(%) 1.2

1/1 1/2 2/1 2/2 3/1 3/2

1.5 1.5 1.5 1.5 1.5 1.5

0.651 0.651 0.651 0.651 0.651 0.651 MEAN

101.7 103.4

102.6

97.0 97.0 96.2 98.7 99.0

97.0

0.0

0.0

97.5

1.8

1.8

1.3

Overall RSD r

Carnitine Day/

Fortification (mg/100g)

Innate

Marginal Recovery

MEAN

SD (%) 3.1

RSD r

Replicate

(mg/100g)

(%)

(%)

(%) 2.9

1/1 1/2 2/1 2/2 3/1 3/2

0.16 0.16 0.16 0.16 0.16 0.16

104.0 108.4 103.9 102.7

106.2

103.3

0.8

0.8

97.9 92.9

95.4

3.5

3.7

101.6

2.8

Overall RSD r

Repeatability The repeatability RSD r

of the method was obtained through analysis of all 17 SPIFAN test kit materials over at least four days in triplicate. Powders were reconstituted fresh for each analysis. The working standard levels were prepared fresh each analysis. Each sample was analyzed by at least two different analysts, with a total of four different analysts used to generate the precision and accuracy data. Two different instruments and two different column lots were used. Results that calculated to be outliers based on a 95% confidence interval using Grubb’s outlier test were replaced with re-analysis to obtain 12 data points overall for each product. Repeatability for the lower level of the analytical range can be found in the LOQ tests in Tables 10 and 11 and the upper level of the analytical range in Table 16 for choline due to the absence of products with this high of an amount. Overall summary tables are provided that give the repeatability of the method over the analytical range (Tables 12-15). The results obtained meet the requirements of the SMPR for total choline and carnitine.