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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
25
SD
0.4
0.0
5.9
% RSD
5.0
0.2
5.8
Th e spike recovery evaluation for vitamin K1 on the second day of the trial was performed at a higher
spike levels (6.0-6.5 mcg/100g) and was found to be in the range of 99.1-103.9% 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 2.9-5.8%
An average summary of the % spike recovery in replicates on two separate days are provided in Table
7c.
Table 7c: Vitamin K1 Spike recovery in SPIFAN matrices on multiple days
VIT K1 Spike Recovery Parameters
% Recovery
Day 1
Day 2
average:
96.7
100.0
Stdev:
4.9
5.3
%RSD:
5.1
5.3
n:
29
15
Spike Recovery Parameters
% Recovery
Average of both
days for all
replicates
average:
97.8
Stdev:
5.2
%RSD:
5.4
n:
44
An average of the spike recovery for vitamin K1 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
7c. An average spike recovery of 97.8% was obtained with range of 96.1-100.0% 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 5.1-5.4%
Vitamin K1 recovery was tried at different spike levels. The data presented in Table 7 don’t
differentiate vitamin K1 recovery at different spike levels. Average of vitamin K1 recovery obtained at
different spike levels in triplicates of different SPIFAN samples is presented in Table 7d.
Table 7d: Vitamin K1 recovery obtained in different SPIFAN samples at different spike levels
Sample
Spike Level I (1.5-
2.0 mcg/100g)
Spike Level II
(2.5-3.0
mcg/100g)
Spike level III (6-
6.5 mcg/100g)
1
95.5
92.1
93.9
2
102.6
94
103.6
3
97.8
94
99.1
VitK-01 w/SLV
FOR ERP USE ONLY
DO NOT DISTRIBUTE