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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
24
% RSD
4.5
0.1
4.5
Mean
1.9
2.5
4.0
4.4
92.0
3
SD
0.1
0.0
1.5
% RSD
1.7
0.4
1.7
The spike recovery for vitamin K1 on the first day of trial at all of the investigated spike levels was
found to be in the range of 92.1-102% 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 1.7-5.4%.
Vitamin K1 spike recovery evaluation in the SPIFAN samples was repeated on a second day at a higher
spike levels (6.0-6.5 mcg/100g) and the results are presented in Table 7b.
Table 7b: Vitamin K1 Spike recovery in SPIFAN matrices on multiple days, Day 2 data
VITAMIN K1
Day 2
Sample Parameters
Sample
ng/g
spike
amt n/g
(approx)
Obtained
(ng/g)
Expected
(ng/g)
%
Recovery
n
1
Mean
2.0
6.0
7.4
7.9
93.9
3
SD
0.3
0.1
4.6
% RSD
4.3
0.8
4.9
2
Mean
1.8
6.0
8.0
7.7
103.6
3
SD
0.3
0.0
3.5
% RSD
3.4
0.4
3.3
3
Mean
3.7
6.0
9.5
9.6
99.1
3
SD
0.3
0.0
2.9
% RSD
3.0
0.2
2.9
4
Mean
3.6
6.5
10.1
10.0
101.7
3
SD
0.5
0.0
5.9
% RSD
5.4
0.4
5.8
5
Mean
2.2
6.0
7.9
8.1
101.7
3
VitK-01 w/SLV
FOR ERP USE ONLY
DO NOT DISTRIBUTE