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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
22
n
8
8
8
SPIFAN
Sample #12
Mean
7.4
0.9
8.3
Stdev
0.6
0.1
0.6
% RSD
8.1
6.6
7.1
n
9
9
9
SPIFAN
Sample #13
Mean
5.0
1.1
6.1
Stdev
0.6
0.1
0.7
% RSD
11.4
9.8
11.0
n
9
9
9
SPIFAN
Sample #14
Mean
5.4
1.1
6.5
Stdev
0.3
0.1
0.3
% RSD
4.9
10.7
3.9
n
8
8
8
SPIFAN
Sample #15
Mean
7.8
1.4
9.1
Stdev
0.7
0.1
0.8
% RSD
9.4
8.0
8.6
n
9
9
9
SPIFAN
Sample #16
Mean
6.2
2.3
8.5
Stdev
0.5
0.3
0.5
% RSD
7.6
12.5
5.4
n
8
8
8
SPIFAN
Sample #17
Mean
7.7
2.8
10.5
Stdev
0.4
0.2
0.5
% RSD
5.7
5.4
5.0
n
8
8
8
All powder samples reconstituted before the analysis (About 25 in
200 mL water. RF samples analyzed as such.
Concentration of Vitamin K1 (Total, trans + cis) was found to be in the range of 2.6 – 11.5 µg/100g in
the analyzed samples when analyzed third time in replicates. The precision of the vitamin K1 analysis
in terms of the % RSD was estimated to be equal or under 8% in most of the analyzed samples with
concentration of total (trans + cis) vitamin K1 within the range of 1 -10 mcg/100g as stipulated in the
Vitamin K SMPR 2014.001. Some samples however gave some what higher % RSD values (11 -
13%,) in their replicate analysis. The sample with concentration of Vit K1 higher than 10 µg/100g,
provided % RSD values closer to 5%.
Cis –vitamin K1 was always found at relatively lower levels (0.3-2.8 µg/100g) in the samples with a %
RSD of the replicates in the range of 5.0 -12.5 %. 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 2.2 – 10.1 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 value for trans-vitamin K1analysis of the replicates of some of the samples was
some what higher (9.4-15.3%). The sample with concentration of Vit K1 higher than 10 µg/100g
provided % RSD value of 6.2%.
The precision of the method for vitamin K1 analysis can be stated based on the average % RSD value
of all the 12 SPIFAN samples tested in replicates (usually 3) on three different days thus replicates of
usually 8-9 for every sample. The precision of the vitamin K1method based on the average % RSD
VitK-01 w/SLV
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