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

SD

0.4 5.0

0.0 0.2

5.9 5.8

% RSD

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

% Recovery

VIT K1 Spike Recovery Parameters

Day 1

Day 2 100.0

96.7

average:

4.9 5.1

5.3 5.3

Stdev: %RSD:

29

15

n:

% Recovery Average of both days for all replicates

Spike Recovery Parameters

average:

97.8

Stdev: %RSD:

5.2 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

Spike Level II (2.5-3.0 mcg/100g)

Spike Level I (1.5- 2.0 mcg/100g)

Spike level III (6- 6.5 mcg/100g)

Sample

1 2 3

95.5

92.1

93.9

102.6

94 94

103.6

97.8

99.1

Silliker Laboratories, Chemistry Research Center, Date: 1/30/15

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