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

4.5 4.0 0.1 1.7

0.1 4.4 0.0 0.4

4.5

Mean

92.0

SD

1.5 1.7

1.9

2.5

3

% RSD

The spike recovery for vitamin K1 on the first day of trial at all of the investigated spike levels was found to be in the range of 92.1-102% and within the range stipulated by the SMPR. The precision of the spike recovery evaluation in replicates at all spike levels as % RSD was calculated. The values obtained were quite satisfactory and in the range of 1.7-5.4%. Vitamin K1 spike recovery evaluation in the SPIFAN samples was repeated on a second day at a higher spike levels (6.0-6.5 mcg/100g) and the results are presented in Table 7b.

Table 7b: Vitamin K1 Spike recovery in SPIFAN matrices on multiple days, Day 2 data

VITAMIN K1 Day 2

spike amt n/g (approx)

Sample ng/g

Obtained (ng/g)

Expected (ng/g)

% Recovery

Sample Parameters

n

Mean

7.4 0.3 4.3

7.9 0.1 0.8

93.9

SD

4.6 4.9

2.0

6.0

3

% RSD

1

Mean

8.0 0.3 3.4

7.7 0.0 0.4

103.6

SD

3.5 3.3

1.8

6.0

3

% RSD

2

Mean

9.5 0.3 3.0

9.6 0.0 0.2

99.1

SD

2.9 2.9

3.7

6.0

3

% RSD

3

Mean

10.1

10.0

101.7

SD

0.5 5.4

0.0 0.4

5.9 5.8

3.6

6.5

3

% RSD

4

5

Mean

2.2

6.0

7.9

8.1

101.7

3

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

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