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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
28
% RSD
4
Mean
0.0
7.5
7.7
7.4
103.6
3
SD
0.2
0.0
3.7
% RSD
3.1
0.5
3.6
Mean
SD
% RSD
5
Mean
0.3
7.5
7.6
7.7
98.2
3
SD
0.4
0.0
6.0
% RSD
5.9
0.3
6.1
Mean
SD
% RSD
The spike recovery evaluation for vitamin K2-7 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
range stipulated by the SMPR. The precision of the spike recovery evaluation in replicates as % RSD
was calculated. The values obtained were quite satisfactory and in the range of 1.1-6.0%
An average summary of the % spike recovery in replicates on two separate days for vitamin K2-7 is
provided in Table 8c.
Table 8c: Vitamin K2-7 Spike recovery in SPIFAN matrices on multiple days
VIT K2-7 Spike Recovery Parameters
% Recovery
Day 1
Day 2
average:
99.1
100.1
Stdev:
5.5
3.7
%RSD:
5.6
3.7
n:
30
15
Spike Recovery Parameters
% Recovery
Average of both
days for all
replicates
average:
99.4
Stdev:
5.0
%RSD:
5.0
n:
45
An average of the spike recovery for vitamin K2-7 obtained in replicate analysis of the analyzed spiked
and non-spiked samples on two separate days at all the investigated spike levels is presented in Table
8c. An average spike recovery of 99.4% with a range of 99.1-100.1% was obtained is within the range
stipulated by the SMPR. The precision of the spike recovery evaluation in replicates as % RSD was
calculated. The values obtained were quite satisfactory and in the range of 3.7-5.6%.
Vitamin K2-4 spike recovery evaluation in the SPIFAN samples was performed by spiking the first five
SPIFAN samples (powder samples reconstituted as liquid, RF samples used as is) with K2-4 at
different spike levels in replicates. The spiked and non-spiked samples were analyzed in replicates
VitK-01 w/SLV
FOR ERP USE ONLY
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