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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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value of all the 12 SPIFAN samples tested in replicates on multiple days is 7.9% (n=300).
% Spike Recovery Evaluation (for accuracy) of the method:
The spike recovery evaluation was performed by spiking the first five SPIFAN samples (powder
samples reconstituted as liquid, RF samples used as is) with Vitamin K1, K2-4 and K2-7 at different
spike levels. The samples were spiked in replicates. Spiked and non-spiked samples were analyzed in
replicates (usually n=3) on two separate days for vitamin K analytes and the spike recovery was
calculated. The results are presented in Tables 7a-c for Vitamin K1, 8a-c Vitamin K2-7, and 9a-c
Vitamin K2-4. The results of the first day of the trial for vitamin K1 spike recovery evaluation are
presented in Table 7a.
Table 7a: Vitamin K1 Spike recovery in SPIFAN matrices on multiple days, Day1 data
VITAMIN K1
Day 1
Sample Parameters mcg/100g
spike amt
mcg/100g
Obtained
(mcg/100g)
Expected
(mcg/100g)
%
Recovery
n
1
Mean
2.0
1.5
3.3
3.5
95.5
2
SD
-
-
-
% RSD
-
-
-
Mean
2.0
3.0
4.5
4.9
92.1
3
SD
0.2
0.0
4.5
% RSD
4.6
0.4
4.9
2
Mean
1.7
1.7
3.5
3.4
102.6
3
SD
0.1
0.0
3.0
% RSD
2.8
0.2
3.0
Mean
1.7
3.0
4.4
4.7
94.0
3
SD
0.2
0.0
4.2
% RSD
4.5
0.6
4.4
3
Mean
3.7
2.0
5.5
5.7
97.8
3
SD
0.2
0.0
2.7
% RSD
2.7
0.1
2.8
Mean
3.7
3.0
6.2
6.6
94.0
3
SD
0.3
0.0
4.9
% RSD
5.5
0.4
5.3
4
Mean
3.1
2.0
5.2
5.1
100.9
3
SD
0.3
0.0
5.4
% RSD
5.3
0.1
5.4
Mean
3.1
3.0
6.2
6.1
101.1
3
SD
0.1
0.0
1.3
% RSD
1.5
0.3
1.3
5
Mean
1.9
1.5
3.3
3.4
96.2
3
SD
0.1
0.0
4.4
VitK-01 w/SLV
FOR ERP USE ONLY
DO NOT DISTRIBUTE