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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
30
The values obtained were quite satisfactory and in the range of 1.9-7.3%.
Vitamin K2-4 spike recovery evaluation in the SPIFAN samples was repeated on a second day at a
higher spike levels (6.5-7.5 mcg/100g) and the results are presented in Table 9b.
Table 9b: Vitamin K2-4 Spike recovery in SPIFAN matrices on multiple days, Day 2 data
VITAMIN K2-4
Day 2
Sample Parametrs
Sample
ng/g
spike
amt n/g
(approx)
Obtained
(ng/g)
Expected
(ng/g)
%
Recovery
n
1
Mean
0.0
6.5
8.2
8.2
100.2
3
SD
0.2
0.1
3.4
% RSD
3.0
0.7
3.4
Mean
SD
% RSD
2
Mean
0.0
7.0
7.0
6.9
100.5
3
SD
0.0
0.0
1.1
% RSD
0.7
0.5
1.1
Mean
SD
% RSD
3
Mean
0.0
7.0
7.0
7.1
98.0
3
SD
0.1
0.0
2.1
% RSD
2.1
0.1
2.1
Mean
SD
% RSD
4
Mean
0.0
7.5
7.7
7.4
103.6
3
SD
0.2
0.0
3.7
% RSD
3.1
0.5
3.6
Mean
SD
% RSD
5
Mean
0.0
7.5
7.6
7.7
98.2
3
SD
0.4
0.0
6.0
% RSD
5.9
0.3
6.1
Mean
SD
% RSD
The spike recovery evaluation for vitamin K2-4 on the second day of the trial was performed at a
higher spike levels (6.5-7.5 mcg/100g) and was found to be in the range of 98.0-103.6% and within the
VitK-01 w/SLV
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