AOAC SPIFAN ERP Meeting Book-March 16, 2016
VitK-01 w/SLV FOR ERP USE ONLY DO NOT DISTRIBUTE
Silliker Chem, Res. Center Crete, IL – Validation of a LC-MS/MS Method for Vitamin K Analysis
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
Total (trans + cis)
Paramtrs
Trans
Cis
Sample ID
mcg/100g of RF sample as is or a powder sample reconstituted in to a liquid
Mean
10.1
1.4 0.1
11.5
0.6 6.2
0.7 6.3
Stdev
SPIFAN Sample #6
10.4
% RSD
8
8
8
n
Mean Stdev
2.2 0.3
1.1 0.1
3.3 0.4
SPIFAN Sample #7
15.3
10.8
13.0
% RSD
7
7
7
n
Mean Stdev
5.9 0.7
1.1 0.1 9.3
7.0 0.8
SPIFAN Sample #8
11.8
11.2
% RSD
8
8
8
n
Mean
7.1 0.4 5.8
1.0 0.1
8.1 0.5 6.1
Stdev
SPIFAN Sample #9
10.1
% RSD
9
9
9
n
Mean Stdev
2.4 0.3
0.3 0.0
2.6 0.3
SPIFAN Sample #10
12.8
11.1
11.0
% RSD
9
9
9
n
Mean
2.2 0.2 7.4
0.4 0.0
2.6 0.2 6.3
SPIFAN Sample #11
Stdev
10.9
% RSD
Silliker Laboratories, Chemistry Research Center, Date: 1/30/15
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