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Silliker
Chem, Res. Center Crete, IL – Validation of a LC-MS/MS Method for Vitamin K Analysis
Silliker Laboratories, Chemistry Research Center, Date: 1/30/15
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RSD of the replicates in the range of 1.7-13.0 %. The lower relative level of the analyte in samples may
be associated with the observed higher variance in the analysis of the replicates.
Trans –vitamin K1 was found to be in the range of 2.1 – 10.3 µg/100g in the analyzed samples. % RSD
of the trans-vitamin K1 analysis was estimated to be under 8% in replicates of many of the analyzed
samples. But % RSD in the trans-vitamin K1analysis of the replicates of some of the samples gave
higher % RSD values in their replicate analysis. . The sample with concentration of Vit K1 higher than
10 µg/100g provided % RSD value of 5% as stipulated in the SMPR.
A summary of the Results for the averages of repeatability/interday-precision (%RSD
r
) for each of the
sample are presented Table 6.
Table 6: Analysis of different SPIFAN samples in replicates on multiple
days – Results of all replicates including those analyzed on different days in replicates
Average of Analysis of replicates on All Three Days
Sample ID
Paramtrs
Trans
Cis
Total
(trans +
cis)
mcg/100g of RF sample as is or a powder
sample reconstituted in to a liquid
SPIFAN
Sample #6
Mean
10.1
1.4
11.5
Stdev
0.6
0.1
0.7
% RSD
6.2
10.4
6.3
n
8
8
8
SPIFAN
Sample #7
Mean
2.2
1.1
3.3
Stdev
0.3
0.1
0.4
% RSD
15.3
10.8
13.0
n
7
7
7
SPIFAN
Sample #8
Mean
5.9
1.1
7.0
Stdev
0.7
0.1
0.8
% RSD
11.8
9.3
11.2
n
8
8
8
SPIFAN
Sample #9
Mean
7.1
1.0
8.1
Stdev
0.4
0.1
0.5
% RSD
5.8
10.1
6.1
n
9
9
9
SPIFAN
Sample #10
Mean
2.4
0.3
2.6
Stdev
0.3
0.0
0.3
% RSD
12.8
11.1
11.0
n
9
9
9
SPIFAN
Sample #11
Mean
2.2
0.4
2.6
Stdev
0.2
0.0
0.2
% RSD
7.4
10.9
6.3
VitK-01 w/SLV
FOR ERP USE ONLY
DO NOT DISTRIBUTE