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

(usually n=3) on two separate days for vitamin K2-4 and the spike recovery was calculated. The results are presented in Tables 9a-a-c. The results of the first day of the trial for vitamin K2-4 spike recovery evaluation are presented in Table 9a.

Table 9a: Vitamin K2-4 Spike recovery in SPIFAN matrices on multiple days, Day1 data

VITAMIN K2-4 Day 1

Sample mcg/100g

spike amt mcg/100g

Obtained (mcg/100g)

Expected (mcg/100g)

% Recovery

Sample

n

Parametrs

1.4 0.1 6.9 2.7 0.0 1.4 1.6 0.1 3.5 2.8 0.1 4.0 1.5 0.0 2.1 2.5 0.2 6.7 1.4 0.0 1.6 2.6 0.2 6.5 1.6 0.0 2.6 2.4 0.1 4.9

1.5 0.0 0.5 2.9 0.0 0.7 1.6 0.0 0.4 3.0 0.0 0.9 1.5 0.0 0.3 2.5 0.0 1.0 1.5 0.0 0.1 2.7 0.0 0.6 1.6 0.0 0.0 2.5 0.0 0.7

93.3

SD

6.8 7.3

0.0

1.5

2

% RSD

1

Mean

91.8

SD

1.7 1.9

0.0

3.0

3

% RSD

Mean

102.3

SD

0.0

1.6

3.5 3.5

3

% RSD

2

Mean

94.7

SD

3.7 3.9

0.0

3.0

3

% RSD

Mean

102.7

SD

0.0

1.5

2.5 2.4

3

% RSD

3

Mean

99.3

SD

5.6 5.7

0.0

2.5

3

% RSD

Mean

96.1

SD

0.0

1.5

1.5 1.5

3

% RSD

4

Mean

96.2

SD

6.7 6.9

0.0

2.7

3

% RSD

Mean

98.4

SD

0.0

1.6

2.5 2.6

3

% RSD

5

Mean

97.9

SD

0.0

2.5

4.1 4.2

3

% RSD

The spike recovery for vitamin K2-4 obtained on the first day of the trial at all of the investigated spike levels was found to be in the range of 91.8-102.7% and is within the range stipulated by the SMPR. The precision of the spike recovery evaluation in replicates at all spike levels as % RSD was calculated.

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

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