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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
27
% RSD
5.3
0.8
4.5
4
Mean
0.0
1.5
1.5
1.5
101.3
3
SD
0.0
0.0
2.4
% RSD
2.3
0.1
2.4
Mean
-
3.0
3.0
3.0
98.8
SD
0.3
0.0
10.6
% RSD
10.3
0.6
10.7
5
Mean
0.3
1.5
1.8
1.8
103.0
3
SD
0.1
0.0
3.7
% RSD
3.6
0.1
3.6
Mean
0.3
2.5
2.7
2.8
96.1
SD
0.1
0.0
3.4
% RSD
3.6
0.6
3.5
The spike recovery for vitamin K2-7 obtained on the first day of the trial at all of the investigated spike
levels was found to be in the range of 92.6-103% and within the range stipulated by the SMPR. The
precision of the spike recovery evaluation in replicates at all spike levels as % RSD was calculated. The
values obtained were quite satisfactory and in the range of 1.3-10.7%.
Vitamin K2-7 spike recovery evaluation in the SPIFAN samples was repeated on a second day at a
higher spike levels and the results are presented in Table 8b.
Table 8b Vitamin K2-7 Spike recovery in SPIFAN matrices on multiple days, Day2 data
Sample Parameters
Day 2
Sample
mcg/100g
spike amt
mcg/100g
Obtained
(mcg/100g)
Expected
(mcg/100g)
%
Recovery
n
1
Mean
1.8
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
0.2
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
VitK-01 w/SLV
FOR ERP USE ONLY
DO NOT DISTRIBUTE