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

The values obtained were quite satisfactory and in the range of 1.9-7.3%.

Vitamin K2-4 spike recovery evaluation in the SPIFAN samples was repeated on a second day at a higher spike levels (6.5-7.5 mcg/100g) and the results are presented in Table 9b.

Table 9b: Vitamin K2-4 Spike recovery in SPIFAN matrices on multiple days, Day 2 data

VITAMIN K2-4 Day 2

spike amt n/g (approx)

Sample ng/g

Obtained (ng/g)

Expected (ng/g)

% Recovery

Sample Parametrs

n

Mean

8.2 0.2 3.0

8.2 0.1 0.7

100.2

SD

3.4 3.4

0.0

6.5

3

% RSD Mean SD % RSD

1

Mean

7.0 0.0 0.7

6.9 0.0 0.5

100.5

SD

0.0

7.0

1.1 1.1

3

% RSD Mean SD % RSD

2

Mean

7.0 0.1 2.1

7.1 0.0 0.1

98.0

SD

0.0

7.0

2.1 2.1

3

% RSD Mean SD % RSD

3

Mean

7.7 0.2 3.1

7.4 0.0 0.5

103.6

SD

0.0

7.5

3.7 3.6

3

% RSD Mean SD % RSD

4

Mean

7.6 0.4 5.9

7.7 0.0 0.3

98.2

SD

0.0

7.5

6.0 6.1

3

% RSD Mean SD % RSD

5

The spike recovery evaluation for vitamin K2-4 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

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

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