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
% RSD
Mean
0.0
7.5
7.7 0.2 3.1
7.4 0.0 0.5
103.6
3
SD
3.7 3.6
% RSD Mean SD % RSD
4
Mean
0.3
7.5
7.6 0.4 5.9
7.7 0.0 0.3
98.2
3
SD
6.0 6.1
% RSD Mean SD % RSD
5
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
% Recovery
VIT K2-7 Spike Recovery Parameters
Day 1
Day 2 100.1
99.1
average:
5.5 5.6
3.7 3.7
Stdev: %RSD:
30
15
n:
% Recovery Average of both days for all replicates
Spike Recovery Parameters
average:
99.4
Stdev: %RSD:
5.0 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
Silliker Laboratories, Chemistry Research Center, Date: 1/30/15
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