441 / 696
Table 11. LOQ Total Analysis
Choline
Day/
Fortification
Innate Marginal Recovery
MEAN
SD
RSD
r
Replicate
(mg/100g)
(mg/100g)
(%)
(%)
(%)
(%)
1/1
1.5
0.651
101.7
102.6
1.2
1.2
1/2
1.5
0.651
103.4
2/1
1.5
0.651
97.0
97.0
0.0
0.0
2/2
1.5
0.651
97.0
3/1
1.5
0.651
96.2
97.5
1.8
1.8
3/2
1.5
0.651
98.7
MEAN
99.0
Overall RSD
r
1.3
Carnitine
Day/
Fortification
Innate Marginal Recovery
MEAN
SD
RSD
r
Replicate
(mg/100g)
(mg/100g)
(%)
(%)
(%)
(%)
1/1
0.16
<LOQ
104.0
106.2
3.1
2.9
1/2
0.16
<LOQ
108.4
2/1
0.16
<LOQ
103.9
103.3
0.8
0.8
2/2
0.16
<LOQ
102.7
3/1
0.16
<LOQ
97.9
95.4
3.5
3.7
3/2
0.16
<LOQ
92.9
MEAN
101.6
Overall RSD
r
2.8
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.
Chol-08/Carn-07 (February 2016)
FOR ERP USE ONLY
DO NOT DISTRIBUTE