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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
26
4
100.9
101.1
101.7
5
96.2
92
101.7
Mean
98.6
94.6
100.0
n
15
15
15
SD
3.1
3.7
3.8
% RSD
3.1
4.0
3.8
Vitamin K1 recovery was tried at different spike levels. Average vitamin K1 spike recovery obtained at
spike level I
(1.5-2.0 mcg/100g)
in five different SPIFAN samples 98.6% (n=15). Average vitamin K1
spike recovery obtained at spike level II
(2.5-3.0 mcg/100g)
in five different SPIFAN samples 94.6%
(n=15). Average vitamin K1 spike recovery obtained at spike level III
(6.0-6.5 mcg/100g)
in five
different SPIFAN samples 100% (n=15).
Vitamin K2-7 spike recovery evaluation in SPIFAN samples was performed by spiking the first five
SPIFAN samples (powder samples reconstituted as liquid, RF samples used as is) with K2-7 at
different spike levels in replicates. The spiked and non-spiked samples were analyzed in replicates
(usually n=3) on two separate days for vitamin K2-7 and the spike recovery calculated. The results are
presented in Tables 8a-a-c. The results of the first day of the trial for vitamin K1 spike recovery
evaluation are presented in Table 7a.
Table 8a Vitamin K2-7 Spike recovery in SPIFAN matrices on multiple days, Day1 data
VITAMIN K2-7
Sample Parameters
Day 1
Sample
mcg/100g
spike amt
mcg/100g
Obtained
(mcg/100g)
Expected
(mcg/100g)
%
Recovery
n
1
Mean
2.0
1.5
3.5
3.5
100.3
3
SD
0.3
0.0
9.8
% RSD
9.6
0.2
9.8
Mean
2.0
3.0
5.0
4.9
101.9
SD
0.2
0.0
4.6
% RSD
4.3
0.4
4.5
2
Mean
0.0
1.7
1.7
1.7
100.7
3
SD
0.0
0.0
1.4
% RSD
1.1
0.3
1.3
Mean
0.0
3.2
3.1
3.2
97.5
SD
0.2
0.0
5.1
% RSD
5.9
0.9
5.2
3
Mean
0.3
1.7
1.9
1.9
98.4
3
SD
0.0
0.0
2.5
% RSD
2.4
0.3
2.6
Mean
0.3
3.0
2.8
3.0
92.6
SD
0.1
0.0
4.1
VitK-01 w/SLV
FOR ERP USE ONLY
DO NOT DISTRIBUTE