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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
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(usually n=3) on two separate days for vitamin K2-4 and the spike recovery was calculated. The results
are presented in Tables 9a-a-c. The results of the first day of the trial for vitamin K2-4 spike recovery
evaluation are presented in Table 9a.
Table 9a: Vitamin K2-4 Spike recovery in SPIFAN matrices on multiple days, Day1 data
VITAMIN K2-4
Day 1
Sample
Parametrs
Sample
mcg/100g
spike amt
mcg/100g
Obtained
(mcg/100g)
Expected
(mcg/100g)
%
Recovery
n
1
0.0
1.5
1.4
1.5
93.3
2
SD
0.1
0.0
6.8
% RSD
6.9
0.5
7.3
Mean
0.0
3.0
2.7
2.9
91.8
3
SD
0.0
0.0
1.7
% RSD
1.4
0.7
1.9
2
Mean
0.0
1.6
1.6
1.6
102.3
3
SD
0.1
0.0
3.5
% RSD
3.5
0.4
3.5
Mean
0.0
3.0
2.8
3.0
94.7
3
SD
0.1
0.0
3.7
% RSD
4.0
0.9
3.9
3
Mean
0.0
1.5
1.5
1.5
102.7
3
SD
0.0
0.0
2.5
% RSD
2.1
0.3
2.4
Mean
0.0
2.5
2.5
2.5
99.3
3
SD
0.2
0.0
5.6
% RSD
6.7
1.0
5.7
4
Mean
0.0
1.5
1.4
1.5
96.1
3
SD
0.0
0.0
1.5
% RSD
1.6
0.1
1.5
Mean
0.0
2.7
2.6
2.7
96.2
3
SD
0.2
0.0
6.7
% RSD
6.5
0.6
6.9
5
Mean
0.0
1.6
1.6
1.6
98.4
3
SD
0.0
0.0
2.5
% RSD
2.6
0.0
2.6
Mean
0.0
2.5
2.4
2.5
97.9
3
SD
0.1
0.0
4.1
% RSD
4.9
0.7
4.2
The spike recovery for vitamin K2-4 obtained on the first day of the trial at all of the investigated spike
levels was found to be in the range of 91.8-102.7% and is within the range stipulated by the SMPR.
The precision of the spike recovery evaluation in replicates at all spike levels as % RSD was calculated.
VitK-01 w/SLV
FOR ERP USE ONLY
DO NOT DISTRIBUTE