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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
20
SPIFAN
Sample #9
Mean
7.3
0.9
8.3
Stdev
0.3
0.1
0.6
% RSD
3.7
9.5
7.2
n
3
2
9
SPIFAN
Sample #10
Mean
2.1
0.3
2.4
Stdev
0.3
0.0
0.3
% RSD
12.7
13.0
10.8
n
3
2
3
SPIFAN
Sample #11
Mean
2.1
0.4
2.5
Stdev
0.2
0.0
0.2
% RSD
10.5
8.1
7.2
n
2
2
2
SPIFAN
Sample #12
Mean
7.3
0.9
8.1
Stdev
0.1
0.1
0.0
% RSD
0.8
8.7
0.6
n
3
3
3
SPIFAN
Sample #13
Mean
5.1
1.1
6.2
Stdev
0.6
0.1
0.7
% RSD
12.5
7.7
11.6
n
3
3
3
SPIFAN
Sample #14
Mean
5.2
1.2
6.4
Stdev
0.2
0.1
0.3
% RSD
4.8
9.7
4.9
n
3
3
3
SPIFAN
Sample #15
Mean
8.2
1.4
9.6
Stdev
1.1
0.1
1.2
% RSD
13.7
8.4
12.7
n
3
3
3
SPIFAN
Sample #16
Mean
5.9
2.5
8.4
Stdev
0.5
0.2
0.5
% RSD
8.4
6.0
5.8
n
3
3
3
SPIFAN
Sample #17
Mean
7.7
3.0
10.7
Stdev
0.4
0.1
0.5
% RSD
5.2
4.7
5.0
n
2
2
2
All powder samples reconstituted before the analysis (About 25 in 200 mL water). RF samples analyzed
as such.
Concentration of Vitamin K1 (Total, trans + cis) was found to be in the range of 2.1 – 10.3 µg/100g in
the analyzed samples when analyzed third time in replicates. The precision of the vitamin K1 analysis
in terms of the % RSD was estimated to be equal or under 8% in most of the analyzed samples with
concentration of total (trans + cis) vitamin K1 within the range of 1 -10 mcg/100g as stipulated in the
Vitamin K SMPR 2014.001. Some samples however gave % RSD values some what higher values
(10.8%, 11.6% and 12.7%) in their replicate analysis. The sample with concentration of Vit K1 higher
than 10 µg/100g, provided % RSD values closer to 5%.
Cis –vitamin K1 was always found at relatively lower levels (0.4-3.0 µg/100g) in the samples with a %
VitK-01 w/SLV
FOR ERP USE ONLY
DO NOT DISTRIBUTE