AOAC SPIFAN ERP Meeting Book-March 16, 2016
VitK-01 w/SLV FOR ERP USE ONLY DO NOT DISTRIBUTE
Silliker Chem, Res. Center Crete, IL – Validation of a LC-MS/MS Method for Vitamin K Analysis
The values obtained were quite satisfactory and in the range of 1.9-7.3%.
Vitamin K2-4 spike recovery evaluation in the SPIFAN samples was repeated on a second day at a higher spike levels (6.5-7.5 mcg/100g) and the results are presented in Table 9b.
Table 9b: Vitamin K2-4 Spike recovery in SPIFAN matrices on multiple days, Day 2 data
VITAMIN K2-4 Day 2
spike amt n/g (approx)
Sample ng/g
Obtained (ng/g)
Expected (ng/g)
% Recovery
Sample Parametrs
n
Mean
8.2 0.2 3.0
8.2 0.1 0.7
100.2
SD
3.4 3.4
0.0
6.5
3
% RSD Mean SD % RSD
1
Mean
7.0 0.0 0.7
6.9 0.0 0.5
100.5
SD
0.0
7.0
1.1 1.1
3
% RSD Mean SD % RSD
2
Mean
7.0 0.1 2.1
7.1 0.0 0.1
98.0
SD
0.0
7.0
2.1 2.1
3
% RSD Mean SD % RSD
3
Mean
7.7 0.2 3.1
7.4 0.0 0.5
103.6
SD
0.0
7.5
3.7 3.6
3
% RSD Mean SD % RSD
4
Mean
7.6 0.4 5.9
7.7 0.0 0.3
98.2
SD
0.0
7.5
6.0 6.1
3
% RSD Mean SD % RSD
5
The spike recovery evaluation for vitamin K2-4 on the second day of the trial was performed at a higher spike levels (6.5-7.5 mcg/100g) and was found to be in the range of 98.0-103.6% and within the
Silliker Laboratories, Chemistry Research Center, Date: 1/30/15
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